CN101728044B - Method for preparing gold magnetic particles - Google Patents
Method for preparing gold magnetic particles Download PDFInfo
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- CN101728044B CN101728044B CN200910219500A CN200910219500A CN101728044B CN 101728044 B CN101728044 B CN 101728044B CN 200910219500 A CN200910219500 A CN 200910219500A CN 200910219500 A CN200910219500 A CN 200910219500A CN 101728044 B CN101728044 B CN 101728044B
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Abstract
The invention belongs to the field of composite material synthesis, relating to a method for preparing composite material of gold coated magnetic oxide, i.e. gold magnetic particles, in particular to a method for preparing the gold magnetic particles by utilizing positive micro-emulsion and a one-step synthesis method. The method comprises the following steps of: establishing a positive micro-emulsion system by taking an organic reagent dispersed with oil-soluble magnetic oxide as cores and oil phase of the gold magnetic particles; then taking emulsion as a microreactor for producing the composite materials; and adding ethanol for demulsification after reaction; separating and washing the magnetic composite particles by utilizing a magnetic separator to prepare the gold magnetic particles. The method has mild reaction conditions, simple preparation process and water-soluble reagent, can be conveniently applied and is easy to realize large-scale production. AuC14- of chlorogold acid is adsorbed at the surface of the oil-soluble oxide particles by a cation surface active agent selected in the method for further reduction, reunion of the composite is little, and the coating is uniform. The sizes of the particles are controlled by controlling the size of the microreactor, and the sizes of the particles are uniform.
Description
Technical field
The invention belongs to the synthetic field of composite material, relate to a kind of composite material of gold-coating magnetic property oxide, i.e. the preparation method of gold-magnetic particles particularly a kind ofly prepares gold-magnetic particles with forward microemulsion one-step synthesis.
Background technology
Surface coated magnetic composite particle is the focus of material science research always.Suitable clad material can improve or optimize the physicochemical property of magnetic particle, makes it possess more characteristic, has enlarged the range of application of particulate.The composite material of gold-coating magnetic property oxide becomes the focus that people pay close attention in recent years; Patent ZL03124061.5 and ZL 03153486.4 disclose the preparation method and the application of this composite material; Be named as after the composite particles that this gold and oxide particle combine " gold-magnetic particles "; Because gold utensil is equipped with good biomolecule mobilization capacity, optical property, possesses the separable character of magnetic oxide again, therefore good application prospects is arranged in fields such as biomedicine, electromagnetism; Promoted the research of people to its preparation method, wherein controllable size, homogeneous, polymolecularity are a great problems of this gold-magnetic particles of preparation.Microemulsion method is to make in two kinds of immiscible solution a kind of form with fine droplet be scattered in another to form emulsion in mutually, and the microreactor that generates as composite material with emulsion is then controlled proterties, particle size distribution and the composition of particulate.
Patent 200710159171.9 discloses silver-nickel core-shell particles and has adopted the preparation of microemulsion method; Patent ZL 03124061.5 and ZL 03153486.4 disclose the preparation method and the application of gold/magnetic oxide composite particles; Article J.AM.CHEM.SOC.2007; 129,8698-8699 has also reported the preparation method of this inorganic composite materials, but the above forward microemulsion method that all do not adopt.
Summary of the invention
The object of the present invention is to provide the gentle forward microemulsion method of a kind of reaction condition to prepare the method for gold-magnetic particles.
Technical scheme of the present invention
The preparation method of gold-magnetic particles of the present invention, its special character is: this method is a kind of forward microemulsion method, is with the organic reagent that is dispersed with oil-soluble oxide particle nuclear and the oil phase as the preparation gold-magnetic particles; Under the effect of cationic surfactant; Or under the acting in conjunction of cationic surfactant and cosurfactant, forming the forward microemulsion system with the water that contains gold chloride, the microreactor that generates as gold-magnetic particles with microemulsion then adds the reducing agent reaction; After finishing, reaction adds the ethanol breakdown of emulsion; Carry out Magnetic Isolation with magnetic separator, clean, process gold-magnetic particles; The volume ratio that wherein adds oil phase and water is 1: 5～1: 15, and the concentration of cationic surfactant in this microemulsion system is 1～200mmol/L; Said water comprises the deionized water solution that contains gold chloride or the deionized water solution of reducing agent.
The volume ratio of oil phase and water is 1: 5～1: 15, and the concentration of cationic surfactant in this microemulsion system is 1～200mmol/L, and this is to guarantee that this microemulsion system is the condition of forward microemulsion system.
This invention through controlling certain proportioning water, oil, surfactant or add cosurfactant again, the microreactor that utilizes the microemulsion that configures to provide is then prepared the gold-magnetic particles with regular morphology and crystal formation.Add cosurfactant and can better stablize microemulsion system.
According to this method two technical schemes can be provided
Scheme one: prepare a total microemulsion system, after the reduction reaction, breakdown of emulsion obtains gold-magnetic particles.Its detailed process is:
Step 1) prepares microemulsion system
The oil-soluble oxide particle is dispersed in the organic reagent as nuclear and oil phase, adds cationic surfactant, or add cosurfactant, stirring and evenly mixing again; Add the gold chloride deionized water solution of making water again, stir, till forming uniform microemulsion; The volume ratio of oil phase and water is 1: 5～1: 15, and the concentration of the mixture of cationic surfactant or cationic surfactant and cosurfactant in this microemulsion system is 1～200mmol/L;
Step 2) reduction reaction
The deionized water solution that will contain reducing agent drops in the above-mentioned microemulsion system stirring reaction 3～6 hours under the ultrasonic agitation condition;
The step 3) breakdown of emulsion
After reaction finishes, add ethanol, stir breakdown of emulsion, the Magnetic Isolation supernatant discarded is used washed with de-ionized water again, obtains gold-magnetic particles.
Scheme two: prepare three microemulsion systems respectively, wherein contain oil-soluble oxide particle among the system I, all contain cationic surfactant among system I, II and the III, contain the AuCl of gold chloride among the system II
4 -, contain reducing agent among the system III, system II is added among the system I react, add system III reaction again, so just formed total microemulsion system, accomplished reduction in the course of reaction, breakdown of emulsion obtains gold-magnetic particles again.
Its detailed process is:
Step 1) is set up microemulsion system I
With the organic reagent that is dispersed with oil-soluble oxide particle is nuclear and oil phase, is water with the deionized water, adds cationic surfactant, or adds cosurfactant again, through stirring ultrasonic formation microemulsion system I;
Step 2) sets up microemulsion system II
With the organic reagent is oil phase, is water with the gold chloride deionized water solution, adds cationic surfactant, or adds cosurfactant again, through stirring ultrasonic formation microemulsion system II;
Step 3) is set up microemulsion system III
With the organic reagent is oil phase, is water with the reducing agent deionized water solution, adds cationic surfactant, or adds cosurfactant again, through stirring ultrasonic formation microemulsion system III;
The step 4) reaction
Microemulsion system II is added under stirring condition among the microemulsion system I, reacted 30 minutes～2 hours, again microemulsion system III is dropped under stirring condition in the above-mentioned reaction, continue reaction 1～6 hour.The volume ratio of oil phase and water is 1: 5～1: 15 in this overall reaction system, and the concentration of the mixture of cationic surfactant or cationic surfactant and cosurfactant in this microemulsion system is 1～200mmol/L;
The step 5) breakdown of emulsion
Add ethanol again, stir breakdown of emulsion, the Magnetic Isolation supernatant discarded is used washed with de-ionized water again, obtains gold-magnetic particles.
Organic reagent described in above-mentioned all schemes comprises cyclohexane, n-hexane, toluene or chloroform; Cationic surfactant comprises DTAC, softex kw, stearyl dimethyl benzyl ammonium chloride, four octyl group ammonium bromides; Cosurfactant is the short-chain hydrocarbons reagent of alcohols/thio-alcohol, comprises n-butanol, n-amyl alcohol or n-amyl mercaptan; Reducing agent comprises hydroxylamine hydrochloride, sodium borohydride, trisodium citrate or hydrazine hydrate.
Above-mentioned oil-soluble oxide particle is Fe
3O
4Or γ-Fe
2O
3, particle diameter is 3nm～50nm.
Advantage of the present invention
1, the invention provides a kind of new method for preparing gold-magnetic particles, i.e. forward microemulsion method.
2, this method reaction condition is gentle, and preparation technology is simple, and reactant is water-soluble, can conveniently use like this and the production of easy realization large-scale industrialization.
3, used cationic surfactant makes the AuCl of gold chloride among the present invention
4 -Be adsorbed on the surface of oil-soluble oxide particle, and then reduction, can make compound reunite less, coat evenly like this.
4, can control the size of particle through the size of control microreactor, and size is even.
Description of drawings
The electromicroscopic photograph of the gold-magnetic particles that Fig. 1 prepares for this method.
The uv absorption spectra of the gold-magnetic particles that Fig. 2 prepares for this method.
The saturation magnetization figure of the gold-magnetic particles that Fig. 3 prepares for this method.
Embodiment
Below in conjunction with specific embodiment the present invention is further described, these embodiment do not limit protection scope of the present invention.
Embodiment 1
A kind of each reagent of forward microemulsion and proportioning such as following table:
| Component | Reagent name | The amount of reagent |
| 1. oil phase | The toluene that contains the 0.5g oxide particle | 20ml |
| 2. water | Contain 10% gold chloride deionized water solution | 200ml |
| 3. surfactant | DTAC | 0.5g |
| 4. reducing agent | The 1M hydroxylamine hydrochloride | 10ml |
Concrete steps are following:
Component in the last table 1 and component 3 were mixed 10 minutes; Add component 2 again and continue reaction formation in 40 minutes microemulsion, again component 4 is dropwise added, reacted 5 hours; Add 200ml ethanol and stir ultrasonic 5 minutes breakdowns of emulsion; Reactant placed carry out Magnetic Isolation on the magnet, supernatant is discarded, water cleans and can obtain the gold-magnetic particles that particle diameter is about 60nm 3 times again.
Embodiment 2
A kind of each reagent of forward microemulsion and proportioning such as following table:
| Component | Reagent name | The amount of reagent |
| 1. oil phase | The cyclohexane that contains the 0.5g oxide particle | 20ml |
| 2. water | Contain 10% gold chloride deionized water solution | 200ml |
| 3. surfactant | Stearyl dimethyl benzyl ammonium chloride | 0.5g |
| 4. reducing agent | The 1M hydroxylamine hydrochloride | 10ml |
| 5. cosurfactant | N-amyl mercaptan | 3ml |
Concrete steps are following:
Component in the last table 1 and component 3 were mixed 5 minutes, add component 5 again and continue to stir 5 minutes, add component 2 continuation reactions again and formed microemulsion in 40 minutes; Again component 4 is dropwise added; Reacted 5 hours, and added 200ml ethanol and stir ultrasonic 5 minutes breakdowns of emulsion, reactant is placed carry out Magnetic Isolation on the magnet; Supernatant is discarded, and water cleans and can obtain the gold-magnetic particles that particle diameter is about 60nm 3 times again.
Embodiment 3
A kind of each reagent of forward microemulsion and proportioning such as following table:
Concrete steps are following:
According to listed each component reagent that configures in the last table, stir and form microemulsion, under stirring condition, add microemulsion II among the microemulsion I; Reacted 40 minutes, and again microemulsion III was dropped under stirring condition in the above-mentioned reaction, continue reaction 4 hours; After finishing, reaction adds ethanol, breakdown of emulsion, Magnetic Isolation supernatant discarded; Water cleans again, obtains gold-magnetic particles.
Can find out this method for preparing gold-magnetic particles that from the foregoing description reaction condition is gentle, preparation technology is simple, need not use large-scale instrument and equipment, the gold-magnetic particles good dispersion that it is prepared, and the grain size homogeneous, its electromicroscopic photograph is as shown in Figure 1.Uv absorption spectra is as shown in Figure 2, can find out that from Fig. 2 gold-magnetic particles has good optical property.Saturation magnetization is as shown in Figure 3, and as can beappreciated from fig. 3 gold-magnetic particles has good superparamagnetism.
Claims (5)
1. the preparation method of a gold-magnetic particles, it is characterized in that: this method is a kind of forward microemulsion method, is with the organic reagent that is dispersed with oil-soluble oxide particle nuclear and the oil phase as the preparation gold-magnetic particles; Under the effect of cationic surfactant; Or under the acting in conjunction of cationic surfactant and cosurfactant, forming the forward microemulsion system with the water that contains gold chloride, the microreactor that generates as gold-magnetic particles with microemulsion then adds the reducing agent reaction; After finishing, reaction adds the ethanol breakdown of emulsion; Carry out Magnetic Isolation with magnetic separator, clean, process gold-magnetic particles; The volume ratio that wherein adds oil phase and water is 1: 5～1: 15, and the concentration of cationic surfactant in this microemulsion system is 1～200mmol/L; Said water comprises the deionized water solution that contains gold chloride.
2. the preparation method of gold-magnetic particles according to claim 1, it is characterized in that: the concrete steps of this method are
(1) preparation microemulsion system
The oil-soluble oxide particle is dispersed in the organic reagent as nuclear and oil phase, adds cationic surfactant, or add cosurfactant, stirring and evenly mixing again; Add gold chloride deionized water solution again, stir, till forming uniform microemulsion as water; The volume ratio of oil phase and water is 1: 5～1: 15, and the concentration of the mixture of cationic surfactant or cationic surfactant and cosurfactant in this microemulsion system is 1～200mmol/L;
(2) reduction reaction
The deionized water solution that will contain reducing agent drops in the above-mentioned microemulsion system stirring reaction 3～6 hours under the ultrasonic agitation condition;
(3) breakdown of emulsion
After reaction finishes, add ethanol, stir breakdown of emulsion, the Magnetic Isolation supernatant discarded is used washed with de-ionized water again, obtains gold-magnetic particles.
3. the preparation method of gold-magnetic particles according to claim 1, it is characterized in that: the concrete steps of this method are
(1) sets up microemulsion system I
With the organic reagent that is dispersed with oil-soluble oxide particle is nuclear and oil phase, is water with the deionized water, adds cationic surfactant, or adds cosurfactant again, through stirring ultrasonic formation microemulsion system I;
(2) set up microemulsion system II
With the organic reagent is oil phase, is water with the gold chloride deionized water solution, adds cationic surfactant, or adds cosurfactant again, through stirring ultrasonic formation microemulsion system II;
(3) set up microemulsion system III
With the organic reagent is oil phase, is water with the reducing agent deionized water solution, adds cationic surfactant, or adds cosurfactant again, through stirring ultrasonic formation microemulsion system III;
(4) reaction
Microemulsion system II is added under stirring condition among the microemulsion system I, reacted 30 minutes～2 hours, again microemulsion system III is dropped under stirring condition in the above-mentioned reaction, continue reaction 1～6 hour; The volume ratio of oil phase and water is 1: 5～1: 15 in this overall reaction system, and the concentration of the mixture of cationic surfactant or cationic surfactant and cosurfactant in this microemulsion system is 1～200mmol/L;
(5) breakdown of emulsion
Add ethanol, stir breakdown of emulsion, the Magnetic Isolation supernatant discarded is used washed with de-ionized water again, obtains gold-magnetic particles.
4. according to the described method of the arbitrary claim of claim 1～3, it is characterized in that: said oil phase reagent comprises cyclohexane, n-hexane, toluene or chloroform; Cationic surfactant comprises DTAC, softex kw, stearyl dimethyl benzyl ammonium chloride, four octyl group ammonium bromides; Cosurfactant is the short-chain hydrocarbons reagent of alcohols/thio-alcohol, comprises n-butanol, n-amyl alcohol or n-amyl mercaptan; Reducing agent comprises hydroxylamine hydrochloride, sodium borohydride, trisodium citrate or hydrazine hydrate.
5. method according to claim 4 is characterized in that: said oil-soluble oxide particle is Fe
3O
4Or γ-Fe
2O
3, particle diameter is 3nm～50nm.
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| CN103128307B (en) * | 2013-02-05 | 2015-12-02 | 西安金磁纳米生物技术有限公司 | A kind of preparation method of gold-magnetic particles |
| CN103317143A (en) * | 2013-06-21 | 2013-09-25 | 淮南舜化机械制造有限公司 | Method for preparing boron nitride-gold nanometer composite |
| CN103447547B (en) * | 2013-08-28 | 2015-06-24 | 同济大学 | Method for preparing ferroferric oxide/gold nano-composite particles of star-like structure in micro-emulsion |
| CN105880625B (en) * | 2016-05-04 | 2018-05-25 | 四川大学 | The method that liquid-liquid two-phase method prepares nano-cobalt powder |
| CN106040307B (en) * | 2016-06-06 | 2018-11-27 | 北京科技大学 | One step hydro thermal method synthesizes Fe3O4(PAA) preparation method of@C-Au core-shell structure microballoon |
| CN109608911A (en) * | 2018-11-23 | 2019-04-12 | 华南理工大学 | A kind of fly ash base carbonization modification compounded mix preparation method being filled with for paper |
| CN109434133A (en) * | 2018-12-20 | 2019-03-08 | 江苏经贸职业技术学院 | A kind of synthetic method based on phase transfer method Au nano material |
| CN112986555B (en) * | 2021-02-07 | 2024-05-07 | 武汉生之源生物科技股份有限公司 | GPC-3 chemiluminescence kit |
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| CN101168196A (en) * | 2006-10-27 | 2008-04-30 | 同济大学 | Method for preparing nickel-base amorphous nano particles |
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| CN101168196A (en) * | 2006-10-27 | 2008-04-30 | 同济大学 | Method for preparing nickel-base amorphous nano particles |
Non-Patent Citations (2)
| Title |
|---|
| 刘祖黎等人.超小型Fe3O4/Au纳米复合微粒的制备与表征.《功能材料》.2005,第36卷(第2期),196-199. * |
| 陈葳等人.微乳法制备Au/ Fe2O3,水煤气变换反应催化剂Ⅰ.制备参数对催化剂活性的影响.《催化学报》.2003,第24卷(第11期),第867-871页. * |
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