CN106277066A - A kind of Fe3o4@SiO2the preparation method of magnetic composite - Google Patents

A kind of Fe3o4@SiO2the preparation method of magnetic composite Download PDF

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Publication number
CN106277066A
CN106277066A CN201610628526.3A CN201610628526A CN106277066A CN 106277066 A CN106277066 A CN 106277066A CN 201610628526 A CN201610628526 A CN 201610628526A CN 106277066 A CN106277066 A CN 106277066A
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China
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parts
ethanol solution
mixed material
tetraethyl orthosilicate
dehydrated alcohol
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CN201610628526.3A
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Inventor
张寒冰
童张法
唐艳葵
覃岳隆
宋振宇
张蕾
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Guangxi University
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Guangxi University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide [Fe3O4]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/745Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/33Electric or magnetic properties
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Iron (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

A kind of Fe3O4@SiO2The preparation method of magnetic composite, comprises the steps: that (1) is configured to ethanol containing ammonia;(2) tetraethyl orthosilicate ethanol solution it is configured to;(3) by Fe3O4It is mixed to get the first mixed material with sodium citrate, then in the first mixed material, adds dehydrated alcohol and deionized water, ultrasonic disperse, obtain Fe3O4Disperse system;(4) again tetraethyl orthosilicate ethanol solution and ethanol containing ammonia are gradually dropped Fe simultaneously3O4Disperse system, in course of reaction, is made temperature of reaction system maintain 68 DEG C by Microwave-assisted firing, and carries out lasting mechanical agitation, and the response time is 20min;(5) products therefrom is centrifuged separating, and washing, after vacuum drying, obtains Fe3O4@SiO2, it is stored in drying tower.The inventive method cost is relatively low and easily obtains, simple to operate, and to environment, will not meet the requirement of green syt.

Description

A kind of Fe3O4@SiO2The preparation method of magnetic composite
Technical field
The present invention relates to the preparation field of magnetic composite, specifically a kind of Fe3O4@SiO2The system of magnetic composite Preparation Method.
Background technology
In recent years, Fe3O4Magnetic nano-particle is owing to being provided simultaneously with the double dominant of magnetic-particle and nano-particle, It is widely used in the biomedical sectors such as target medicine carrier, cell separation, nuclear magnetic resonance, NMR, immunoassay, nucleic acid hybridization.With Time, this superparamagnetic material also has good application prospect at catalytic field, can be as liquid phase small size catalyst Catalytic carrier, improves catalyst and separates difficult situation.But Fe3O4Magnetic nano-particle is oxidizable, and specific surface area is higher, has Strong gathering tendency, it is difficult to directly apply.Use unformed SiO2To Fe3O4Magnetic nano-particle carries out Surface coating, SiO2 Clad adds its chemical stability, meanwhile, SiO2Avirulence and the existence of surface hydroxyl improve its biocompatibility, Widen Fe3O4Magnetic nano-particle is in the application in the fields such as biology, catalysis.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that a kind of Fe3O4@SiO2The preparation method of magnetic composite.
To achieve these goals, present invention employs techniques below scheme:
A kind of Fe3O4@SiO2The preparation method of magnetic composite, comprises the steps:
(1) according to volume parts meter, by ammonia that 1 part of mass fraction is 25% and 1.8~2.2 parts of dehydrated alcohol mixing, It is configured to ammonia-ethanol solution;
(2) according to volume parts meter, by 1 part of tetraethyl orthosilicate and 8~12 parts of dehydrated alcohol mixing, it is configured to positive silicic acid second Ester-ethanol solution;
(3) first count by weight, by 0.8~1.2 part of Fe3O4It is mixed to get first with 0.8~1.2 part of sodium citrate to mix Compound material, adds 240~260mL dehydrated alcohol and the ratio of 240~260mL deionized waters according still further to every gram of first mixed material In the first mixed material, add dehydrated alcohol and deionized water, ultrasonic disperse 10~12min, obtain Fe3O4Disperse system;
(4) first according to volume parts meter, measure respectively 13~17 parts of ammonia-ethanol solution, 10~12 parts of tetraethyl orthosilicates- Ethanol solution and 220~280 parts of Fe3O4Disperse system, then by tetraethyl orthosilicate-ethanol solution and ammonia-ethanol solution simultaneously by Gradually instill Fe3O4Disperse system, in course of reaction, is made temperature of reaction system maintain 68~72 DEG C by Microwave-assisted firing, and carries out Lasting mechanical agitation, the response time is 20~30min;
(5) products therefrom is centrifuged separating, and washing, after vacuum drying, obtains Fe3O4@SiO2Magnetic composite, protects It is stored in drying tower.
Described Fe3O4It is prepared by the following method:
(1) count by weight, by 120~150 parts of FeCl3·6H2O, 340~380 parts of CH3COONa and 10~20 parts Sodium citrate mix homogeneously obtains the second mixed material, adds 8~10 milliliters of ethylene glycol according still further to every gram of second mixed material Bulking value ratio adds ethylene glycol in the second mixed material, is uniformly mixing to obtain mixed liquor;
(2) being transferred to by mixed liquor in politef hydrothermal reaction kettle, making reactor is 190~210 DEG C in temperature Muffle furnace heats 8~10h, is then centrifuged for separating, washing, is dried, obtains monodispersed Fe3O4Nano material.
Compared with prior art, the beneficial effect that the present invention possesses:
The Fe that the present invention is prepared3O4@SiO2Magnetic composite is with Fe3O4For magnetic core, coated Si O2Protective layer, has concurrently SiO2The feature such as good biocompatibility, chemical stability, overcomes Fe3O4Owing to dimensional effect, dipole moment gravitation etc. are made Determination with the particle caused easily agglomerate poor stability;And the inventive method cost is relatively low and easily obtains, simple to operate, and And the requirement of green syt to environment, will not be met.
Detailed description of the invention
Below by embodiment, technical scheme is further elaborated.
Embodiment 1
A kind of Fe3O4@SiO2The preparation method of magnetic composite, comprises the steps:
(1) ammonia that 5mL mass fraction is 25% and 10ml dehydrated alcohol are joined it is mixed and made into ammonia-ethanol solution;
(2) 1mL tetraethyl orthosilicate and 10ml dehydrated alcohol are hybridly prepared into tetraethyl orthosilicate-ethanol solution;
(3) 0.2g Fe is weighed3O4Be placed in beaker with 0.2g sodium citrate, add 100mL dehydrated alcohol and 100mL go from Sub-water, ultrasonic disperse 10min, Microwave-assisted firing makes temperature of reaction system maintain 70 DEG C, by tetraethyl orthosilicate-ethanol solution Being gradually dropped with ammonia-ethanol solution, course of reaction carries out lasting mechanical agitation simultaneously, and the response time is 30min;
(4) products therefrom carries out heart separation, and by some times of deionized water, washing with alcohol, after vacuum drying 3h, collects End-product Fe3O4@SiO2Magnetic composite is in drying tower, in order to follow-up preparation uses.
Described Fe3O4It is prepared by the following method:
(1) precise 1.35g FeCl3·6H2O、3.6g CH3COONa and 0.15g sodium citrate, adds 40mL second Glycol, obtains mixed liquor;
(2) by after mixed liquor high-speed stirred 1h, move to, in the politef hydrothermal reaction kettle that capacity is 50mL, make reaction Still is 200 DEG C of work 8h in Muffle furnace, are then centrifuged for separating, after ethanol and deionized water repeatedly wash, are placed in 70 DEG C of vacuum Drying baker is dried, and obtains monodispersed Fe3O4Nano material, is placed in the sample after dried in drying tower, in order to follow-up reality Test use.
Embodiment 2
A kind of Fe3O4@SiO2The preparation method of magnetic composite, comprises the steps:
(1) according to volume parts meter, by ammonia that 1 part of mass fraction is 25% and 1.8 parts of dehydrated alcohol mixing, it is configured to Ammonia-ethanol solution;
(2) according to volume parts meter, by 1 part of tetraethyl orthosilicate and the mixing of 8 parts of dehydrated alcohol, be configured to tetraethyl orthosilicate- Ethanol solution;
(3) first count by weight, by 0.8 part of Fe3O4It is mixed to get the first mixed material with 0.8 part of sodium citrate, then presses The ratio adding 240mL dehydrated alcohol and 240mL deionized water according to every gram of first mixed material adds in the first mixed material Dehydrated alcohol and deionized water, ultrasonic disperse 10min, obtain Fe3O4Disperse system;
(4) first according to volume parts meter, 13 parts of ammonia-ethanol solution, 10 parts of tetraethyl orthosilicate-ethanol solution are measured respectively And 220 parts of Fe3O4Disperse system, then tetraethyl orthosilicate-ethanol solution and ammonia-ethanol solution are gradually dropped Fe simultaneously3O4Point Dissipate system, in course of reaction, Microwave-assisted firing make temperature of reaction system maintain 68 DEG C, and carry out lasting mechanical agitation, Response time is 20min;
(5) products therefrom is centrifuged separating, and washing, after vacuum drying, obtains Fe3O4@SiO2, it is stored in drying tower.
Described Fe3O4It is prepared by the following method:
(1) count by weight, by 120 parts of FeCl3·6H2O, 340 parts of CH3COONa and 10 parts of sodium citrate mixing are all Even obtain the second mixed material, according still further to every gram of second mixed material add the bulking value ratio of 8~10 milliliters of ethylene glycol to Second mixed material adds ethylene glycol, is uniformly mixing to obtain mixed liquor;
(2) mixed liquor is transferred in politef hydrothermal reaction kettle, makes reactor at the Muffle furnace that temperature is 190 DEG C Middle heating 8h, is then centrifuged for separating, washing, is dried, obtains monodispersed Fe3O4Nano material.
Embodiment 3
A kind of Fe3O4@SiO2The preparation method of magnetic composite, comprises the steps:
(1) according to volume parts meter, by ammonia that 1 part of mass fraction is 25% and 2.2 parts of dehydrated alcohol mixing, it is configured to Ammonia-ethanol solution;
(2) according to volume parts meter, by 1 part of tetraethyl orthosilicate and the mixing of 12 parts of dehydrated alcohol, be configured to tetraethyl orthosilicate- Ethanol solution;
(3) first count by weight, by 1.2 parts of Fe3O4It is mixed to get the first mixed material with 1.2 parts of sodium citrates, then presses The ratio adding 260mL dehydrated alcohol and 260mL deionized water according to every gram of first mixed material adds in the first mixed material Dehydrated alcohol and deionized water, ultrasonic disperse 12min, obtain Fe3O4Disperse system;
(4) first according to volume parts meter, 17 parts of ammonia-ethanol solution, 12 parts of tetraethyl orthosilicate-ethanol solution are measured respectively And 280 parts of Fe3O4Disperse system, then tetraethyl orthosilicate-ethanol solution and ammonia-ethanol solution are gradually dropped Fe simultaneously3O4Point Dissipate system, in course of reaction, Microwave-assisted firing make temperature of reaction system maintain 72 DEG C, and carry out lasting mechanical agitation, Response time is 30min;
(5) products therefrom is centrifuged separating, and washing, after vacuum drying, obtains Fe3O4@SiO2, it is stored in drying tower.
Described Fe3O4It is prepared by the following method:
(1) count by weight, by 150 parts of FeCl3·6H2O, 380 parts of CH3COONa and 20 parts of sodium citrate mixing are all Even obtain the second mixed material, add the bulking value ratio of 10 milliliters of ethylene glycol to second according still further to every gram of second mixed material Mixed material adds ethylene glycol, is uniformly mixing to obtain mixed liquor;
(2) mixed liquor is transferred in politef hydrothermal reaction kettle, makes reactor at the Muffle furnace that temperature is 210 DEG C Middle heating 10h, is then centrifuged for separating, washing, is dried, obtains monodispersed Fe3O4Nano material.

Claims (2)

1. a Fe3O4@SiO2The preparation method of magnetic composite, it is characterised in that comprise the steps:
(1) according to volume parts meter, by ammonia that 1 part of mass fraction is 25% and 1.8~2.2 parts of dehydrated alcohol mixing, preparation Ammonification water-ethanol solution;
(2) according to volume parts meter, by 1 part of tetraethyl orthosilicate and the mixing of 8~12 parts of dehydrated alcohol, be configured to tetraethyl orthosilicate- Ethanol solution;
(3) first count by weight, by 0.8~1.2 part of Fe3O4It is mixed to get the first mixture with 0.8~1.2 part of sodium citrate Material, adds the ratio of 240~260mL dehydrated alcohol and 240~260mL deionized waters to the according still further to every gram of first mixed material One mixed material adds dehydrated alcohol and deionized water, ultrasonic disperse 10~12min, obtains Fe3O4Disperse system;
(4) first according to volume parts meter, 13~17 parts of ammonia-ethanol solution, 10~12 parts of tetraethyl orthosilicate-ethanol are measured respectively Solution and 220~280 parts of Fe3O4Disperse system, then tetraethyl orthosilicate-ethanol solution and ammonia-ethanol solution are gradually dripped simultaneously Enter Fe3O4Disperse system, in course of reaction, is made temperature of reaction system maintain 68~72 DEG C by Microwave-assisted firing, and carries out continuing Mechanical agitation, the response time is 20~30min;
(5) products therefrom is centrifuged separating, and washing, after vacuum drying, obtains Fe3O4@SiO2Magnetic composite, is stored in In drying tower.
2. preparation method as claimed in claim 1, it is characterised in that described Fe3O4It is prepared by the following method:
(1) count by weight, by 120~150 parts of FeCl3·6H2O, 340~380 parts of CH3COONa and 10~20 portions of Fructus Citri Limoniaes Acid sodium mix homogeneously obtains the second mixed material, adds the weight of 8~10 milliliters of ethylene glycol according still further to every gram of second mixed material Volume ratio adds ethylene glycol in the second mixed material, is uniformly mixing to obtain mixed liquor;
(2) mixed liquor is transferred in politef hydrothermal reaction kettle, makes reactor in the Muffle that temperature is 190~210 DEG C Stove heats 8~10h, is then centrifuged for separating, washing, is dried, obtains monodispersed Fe3O4Nano material.
CN201610628526.3A 2016-08-03 2016-08-03 A kind of Fe3o4@SiO2the preparation method of magnetic composite Pending CN106277066A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108187741A (en) * 2018-01-09 2018-06-22 天津大学 More carboxyl magnetic Nano silicon ball solid-borne platinum catalysts and its preparation method and application
CN110439517A (en) * 2019-07-12 2019-11-12 浙江海洋大学 A kind of flooding method suitable for heavy crude reservoir

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101640089A (en) * 2009-07-08 2010-02-03 复旦大学 Super paramagnetism inorganic nanometer microballoon and preparation method thereof
CN105621498A (en) * 2016-03-14 2016-06-01 宁波江东索雷斯电子科技有限公司 Preparation method of monodisperse silicon dioxide/ferroferric oxide magnetic composite particles
CN105712409A (en) * 2014-12-03 2016-06-29 中国科学院宁波材料技术与工程研究所 Preparation method of spherical ferriferrous oxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101640089A (en) * 2009-07-08 2010-02-03 复旦大学 Super paramagnetism inorganic nanometer microballoon and preparation method thereof
CN105712409A (en) * 2014-12-03 2016-06-29 中国科学院宁波材料技术与工程研究所 Preparation method of spherical ferriferrous oxide
CN105621498A (en) * 2016-03-14 2016-06-01 宁波江东索雷斯电子科技有限公司 Preparation method of monodisperse silicon dioxide/ferroferric oxide magnetic composite particles

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YANPING WANG ET AL.: ""Synthesis of Fe3O4@SiO2@ZnO core–shell structured microspheres and microwave absorption properties"", 《ADVANCED POWDER TECHNOLOGY》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108187741A (en) * 2018-01-09 2018-06-22 天津大学 More carboxyl magnetic Nano silicon ball solid-borne platinum catalysts and its preparation method and application
CN110439517A (en) * 2019-07-12 2019-11-12 浙江海洋大学 A kind of flooding method suitable for heavy crude reservoir
CN110439517B (en) * 2019-07-12 2021-09-17 浙江海洋大学 Oil displacement method suitable for heavy oil reservoir

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