CN104353431A - Preparation method of beta-cyclodextrin-modified magnetic nano particles - Google Patents

Preparation method of beta-cyclodextrin-modified magnetic nano particles Download PDF

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CN104353431A
CN104353431A CN201410714076.0A CN201410714076A CN104353431A CN 104353431 A CN104353431 A CN 104353431A CN 201410714076 A CN201410714076 A CN 201410714076A CN 104353431 A CN104353431 A CN 104353431A
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曲玉宁
方升
关会兰
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Tianjin Polytechnic University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
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    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
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    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character

Abstract

The invention relates to a preparation method of beta-cyclodextrin-modified magnetic nano particles. A composite nano microsphere with a nuclear-shell structure is prepared. The composite nano microsphere with certain adsorption property is prepared by synthesizing magnetic ferroferric oxide nano particles by a hydrothermal method, then wrapping the nano particles by a layer of SiO2 by taking sodium silicate obtained by rice shell hydrolysis as a silicon source and modifying the surface by beta-CD. The composite nano microsphere has superparamagnetism with the magnetic particles and has subjective and objective clathration on cyclodextrin supermolecules; the nano microsphere with Fe3O4@SiO2/beta-CD has great action on the environmental pollution treatment aspect under the excellent superparamagnetism and the supermolecule clathration.

Description

A kind of preparation method of magnetic nano-particle of beta-cyclodextrin modified
Technical field
The present invention relates to a kind of preparation of magnetic nano-particle of beta-cyclodextrin modified, be specifically related to the composite nano-microsphere first having prepared a kind of nucleocapsid structure, again β-CD is modified at its surface, obtains the research method with the magnetic Nano microsphere of certain adsorption capacity.
Background technology
The decades in past, magnetic nano-particle has been applied to a lot of different field, as traditional electricity, optics, magnetics etc., comprise magnetic in the application of frontier and assist bio-separation and living things catalysis, poisonous anion, cation and metal biosorption, as arsenic (V), chromium (VI) and U (VI).In addition, magnetic nano-particle shows wide application prospect at biomedical sectors such as magnetic in vivo marker, Cellular tracking, load enzymes.The application of magnetic nano-particle becomes one of noticeable and the most most active current research field.As everyone knows, the cyclodextrin (CDs) represented as second generation supermolecule is the cyclic oligosaccharide that the glucopyranose units of varying number is formed by connecting by α-(1-4) glycosidic bond.Because the glucose unit in cyclodextrin is chair conformation, define intermediate void and the cone barrel structure do not closed of two ends, wherein, all primary hydroxyls are positioned at the side of cone, and all secondary hydroxyls are positioned at the opposite side of cone, so the tubular construction of cyclodextrin is also referred to as frustoconical configuration.Therefore, the outer wall of cyclodextrin has hydrophily, and center cavity is hydrophobic, lipophilic.Due to such feature, cyclodextrin selectively can identify guest molecule, the organic and inorganic guest molecule phase inclusion suitable with some sizes, forms supramolecular system, therefore be widely used in fields such as bio-sensing, medical material, environmental improvements, the parent being subject to researchers looks at.
Problem of environmental pollution faced by current many industrial production removes the dyestuff in sewage.Because a lot of dyestuff has good dissolubility, it is common water pollutant.Some of them azo dyes, some microorganisms can decompose azo (N=N) group, and cause it to form aromatic amine product, their major parts are poisonous carcinogens, can affect hydrobiological existence, cause serious environmental problems.Therefore, the method for dyestuff in industrial wastewater of removing is a great challenge, the solution now applied as absorption, coagulation, biodegradation, chemical degradation and light degradation etc.
Summary of the invention
For realizing experimental program provided by the present invention be:
(1) water heat transfer Fe is adopted 3o 4magnetic nano-particle
First a certain amount of FeCl is taken 36H 2o is placed in beaker, pour a certain amount of ethylene glycol into, room-temperature dissolution, stir and add a certain amount of anhydrous sodium acetate to above-mentioned solution, in autoclave reaction, reaction temperature is 220 DEG C, and the time is that 24h takes out, the black solid of preparation is used absolute ethyl alcohol, washed with de-ionized water respectively, and drying can obtain Fe 3o 4nano particle;
(2) Fe is synthesized 3o 4@SiO 2composite nanoparticle
Take a certain proportion of ethanol and deionized water in round-bottomed flask, by a certain amount of for step (1) Fe cleaned up 3o 4nano particle is evenly dispersed in mixed solution through ultrasonic process, then continues in mixed system, drip a certain amount of sodium silicate solution, passes into CO 2gas, stirs 6-12h under the condition of room temperature, and stop stirring after-applied magnetic field and make nano particle enrichment sucking-off, use deionized water and ethanol rinse respectively, vacuum drying can obtain the Fe of brownish black 3o 4@SiO 2composite nanoparticle;
(3) synthesis of cyclodextrin modified magnetic nano-particle
Taking a certain amount of beta-schardinger dextrin-is dissolved completely in the DMF of 50mL; allow to this solution and add a certain amount of sodium hydride; at room temperature stir and obtain white clear solution; then a certain amount of silane coupler is joined in above-mentioned solution, be placed in the round-bottomed flask that vacuumizes, stir 2-8h under nitrogen protection; reaction temperature is 90 DEG C; after reaction terminates, solution is cooled to room temperature, by the Fe of synthesis in a certain amount of step (2) 3o 4@SiO 2join above-mentioned solution, then to mixed solution and dripping ammoniacal liquor (25%), after then at room temperature the reaction of mixture vigorous stirring being terminated, by magnet by compound particle sucking-off, use DMF, deionized water and ethanol rinse respectively, drying can obtain brownish black Fe 3o 4@SiO 2/ β-CD magnetic composite nanoparticles.
Understand the present invention, below in conjunction with embodiment the present invention done to describing in detail further, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1:
(1) water heat transfer Fe is adopted 3o 4magnetic nano-particle
First the FeCl of 1g is taken 36H 2o is placed in beaker, pours the ethylene glycol of 50ml into, room-temperature dissolution, stir the anhydrous sodium acetate adding 3g to above-mentioned solution, in autoclave reaction, reaction temperature is 220 DEG C, time is that 24h takes out, and the black solid of preparation is used absolute ethyl alcohol, washed with de-ionized water respectively, and drying can obtain Fe 3o 4nano particle;
(2) Fe is synthesized 3o 4@SiO 2composite nanoparticle
Take the ethanol of volume ratio 4: 1 and deionized water in round-bottomed flask, by the Fe cleaned up of step (1) 0.02g 3o 4nano particle is evenly dispersed in mixed solution through ultrasonic process, then continues the sodium silicate solution dripping 10ml in mixed system, passes into CO 2gas, stirs 6-12h under the condition of room temperature, and stop stirring after-applied magnetic field and make nano particle enrichment sucking-off, use deionized water and ethanol rinse respectively, vacuum drying can obtain the Fe of brownish black 3o 4@SiO 2composite nanoparticle;
(3) synthesis of cyclodextrin modified magnetic nano-particle
The beta-schardinger dextrin-taking 2g is dissolved completely in the DMF of 50mL; allow the sodium hydride adding 0.4g to this solution; at room temperature stir and obtain white clear solution; then the silane coupler of 3ml is joined in above-mentioned solution; be placed in the round-bottomed flask that vacuumizes, stir 6h under nitrogen protection, reaction temperature is 90 DEG C; after reaction terminates, solution is cooled to room temperature.By the Fe of synthesis in the step (2) of 0.8g 3o 4@SiO 2join above-mentioned solution, then to mixed solution and dripping ammoniacal liquor (25%), after then at room temperature the reaction of mixture vigorous stirring being terminated, by magnet by compound particle sucking-off, use DMF, deionized water and ethanol rinse respectively, drying can obtain brownish black Fe 3o 4@SiO 2/ β-CD magnetic composite nanoparticles.

Claims (1)

1. a preparation method for the magnetic nano-particle of beta-cyclodextrin modified, concrete steps are as follows:
(1) water heat transfer Fe is adopted 3o 4magnetic nano-particle
First a certain amount of FeCl is taken 36H 2o is placed in beaker, pour a certain amount of ethylene glycol into, room-temperature dissolution, stir and add a certain amount of anhydrous sodium acetate to above-mentioned solution, in autoclave reaction, reaction temperature is 220 DEG C, and the time is that 24h takes out, the black solid of preparation is used absolute ethyl alcohol, washed with de-ionized water respectively, and drying can obtain Fe 3o 4nano particle;
(2) Fe is synthesized 3o 4@SiO 2composite nanoparticle
Take a certain proportion of ethanol and deionized water in round-bottomed flask, by a certain amount of for step (1) Fe cleaned up 3o 4nano particle is evenly dispersed in mixed solution through ultrasonic process, then continues in mixed system, drip a certain amount of sodium silicate solution, passes into CO 2gas, stirs 6-12h under the condition of room temperature, and stop stirring after-applied magnetic field and make nano particle enrichment sucking-off, use deionized water and ethanol rinse respectively, vacuum drying can obtain the Fe of brownish black 3o 4@SiO 2composite nanoparticle;
(3) synthesis of cyclodextrin modified magnetic nano-particle
Taking a certain amount of beta-schardinger dextrin-is dissolved completely in the DMF of 50mL; allow to this solution and add a certain amount of sodium hydride; at room temperature stir and obtain white clear solution; then a certain amount of silane coupler is joined in above-mentioned solution, be placed in the round-bottomed flask that vacuumizes, stir 2-8h under nitrogen protection; reaction temperature is 90 DEG C; after reaction terminates, solution is cooled to room temperature, by the Fe of synthesis in a certain amount of step (2) 3o 4@SiO 2join above-mentioned solution, then to mixed solution and dripping ammoniacal liquor (25%), after then at room temperature the reaction of mixture vigorous stirring being terminated, by magnet by compound particle sucking-off, use DMF, deionized water and ethanol rinse respectively, drying can obtain brownish black Fe 3o 4@SiO 2/ β-CD magnetic composite nanoparticles.
CN201410714076.0A 2014-11-26 2014-11-26 Preparation method of beta-cyclodextrin-modified magnetic nano particles Pending CN104353431A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104861743A (en) * 2015-04-13 2015-08-26 成都石大力盾科技有限公司 Method for improving carbon nanotube dispersibility
CN105195101A (en) * 2015-09-21 2015-12-30 济南大学 Preparation method of beta-cyclodextrin modified nanometer silicon nitride adsorbent
CN105820377A (en) * 2016-06-03 2016-08-03 江苏华昌织物有限公司 Preparation method for load cyclodextrin magnetic graphene
CN107837792A (en) * 2017-12-20 2018-03-27 中国海洋大学 A kind of preparation method of cyclodextrin modified magnetic hollow microcapsules sorbing material
CN107961764A (en) * 2017-11-29 2018-04-27 武汉理工大学 A kind of preparation method of carboxymethyl-beta-cyclodextrin functional magnetic mesoporous silicon microballoon
CN108102449A (en) * 2017-12-06 2018-06-01 中国科学院海洋研究所 A kind of the supermolecule microballoon and its synthetic method of marine pressure alternation sensitivity
CN108452781A (en) * 2018-04-02 2018-08-28 福州大学 The preparation method of core-shell magnetic gamma-cyclodextrin polymer composites and application
CN108620049A (en) * 2018-04-16 2018-10-09 浙江财经大学 A kind of sewage disposal preparation and preparation method thereof
CN108727600A (en) * 2018-06-07 2018-11-02 常州大学 A kind of preparation method of the regular nanoparticle based on beta cyclo dextrin polymer
CN109091678A (en) * 2018-08-21 2018-12-28 南开大学 A kind of preparation method and applications of the super-molecule assembling body for the dual regulation inhibiting tumor invasion and diffusion
CN110327985A (en) * 2019-07-15 2019-10-15 湖南工学院 Hyperbranched cyclodextrin-nano ferroso-ferric oxide heterogeneous catalysis and its preparation method and application
CN111359588A (en) * 2020-02-25 2020-07-03 东华大学 Multifunctional cyclodextrin-based magnetic nanospheres and preparation method and application thereof
CN112058239A (en) * 2020-09-08 2020-12-11 中国农业科学院农业质量标准与检测技术研究所 Cyclodextrin magnetic nano composite material, preparation method and application thereof, and adsorbent
CN114667155A (en) * 2019-11-04 2022-06-24 成长生物科技有限公司 Method for selectively recovering hydrophobic compound

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104861743A (en) * 2015-04-13 2015-08-26 成都石大力盾科技有限公司 Method for improving carbon nanotube dispersibility
CN105195101A (en) * 2015-09-21 2015-12-30 济南大学 Preparation method of beta-cyclodextrin modified nanometer silicon nitride adsorbent
CN105195101B (en) * 2015-09-21 2017-06-23 济南大学 A kind of preparation method of beta cyclodextrin modified nano silicon nitride adsorbent
CN105820377A (en) * 2016-06-03 2016-08-03 江苏华昌织物有限公司 Preparation method for load cyclodextrin magnetic graphene
CN107961764A (en) * 2017-11-29 2018-04-27 武汉理工大学 A kind of preparation method of carboxymethyl-beta-cyclodextrin functional magnetic mesoporous silicon microballoon
CN108102449B (en) * 2017-12-06 2021-01-12 中国科学院海洋研究所 Sea pressure alternation sensitive supermolecule microsphere and its synthesis method
CN108102449A (en) * 2017-12-06 2018-06-01 中国科学院海洋研究所 A kind of the supermolecule microballoon and its synthetic method of marine pressure alternation sensitivity
CN107837792A (en) * 2017-12-20 2018-03-27 中国海洋大学 A kind of preparation method of cyclodextrin modified magnetic hollow microcapsules sorbing material
CN108452781A (en) * 2018-04-02 2018-08-28 福州大学 The preparation method of core-shell magnetic gamma-cyclodextrin polymer composites and application
CN108620049A (en) * 2018-04-16 2018-10-09 浙江财经大学 A kind of sewage disposal preparation and preparation method thereof
CN108620049B (en) * 2018-04-16 2021-03-16 浙江财经大学 Sewage treatment preparation and preparation method thereof
CN108727600A (en) * 2018-06-07 2018-11-02 常州大学 A kind of preparation method of the regular nanoparticle based on beta cyclo dextrin polymer
CN109091678A (en) * 2018-08-21 2018-12-28 南开大学 A kind of preparation method and applications of the super-molecule assembling body for the dual regulation inhibiting tumor invasion and diffusion
CN109091678B (en) * 2018-08-21 2022-01-28 南开大学 Preparation method and application of double-regulation supermolecule assembly for inhibiting tumor invasion and diffusion
CN110327985A (en) * 2019-07-15 2019-10-15 湖南工学院 Hyperbranched cyclodextrin-nano ferroso-ferric oxide heterogeneous catalysis and its preparation method and application
CN114667155A (en) * 2019-11-04 2022-06-24 成长生物科技有限公司 Method for selectively recovering hydrophobic compound
CN111359588A (en) * 2020-02-25 2020-07-03 东华大学 Multifunctional cyclodextrin-based magnetic nanospheres and preparation method and application thereof
CN112058239A (en) * 2020-09-08 2020-12-11 中国农业科学院农业质量标准与检测技术研究所 Cyclodextrin magnetic nano composite material, preparation method and application thereof, and adsorbent

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Application publication date: 20150218