CN109559882A - Amphiphilic hydroxyl magnetic bead and its preparation method and application - Google Patents
Amphiphilic hydroxyl magnetic bead and its preparation method and application Download PDFInfo
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- CN109559882A CN109559882A CN201811473412.1A CN201811473412A CN109559882A CN 109559882 A CN109559882 A CN 109559882A CN 201811473412 A CN201811473412 A CN 201811473412A CN 109559882 A CN109559882 A CN 109559882A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
- G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
- G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
- G01N33/54313—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals the carrier being characterised by its particulate form
- G01N33/54326—Magnetic particles
- G01N33/54333—Modification of conditions of immunological binding reaction, e.g. use of more than one type of particle, use of chemical agents to improve binding, choice of incubation time or application of magnetic field during binding reaction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
- G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
- G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
- G01N33/551—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals the carrier being inorganic
- G01N33/553—Metal or metal coated
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
Abstract
The present invention relates to a kind of amphiphilic hydroxyl magnetic beads and its preparation method and application, and the preparation method is the following steps are included: by Fe3O4Magnetic particles 0.5g~5g, hydrophilic silane dressing agent 1mL~20mL, hydrophobic silane dressing agent 0mL~10mL, catalyst 5mL~20mL and solvent 200mL~2500mL mixing, react at 25~80 DEG C；Black precipitate substance is collected after reaction, and washing is drying to obtain amphiphilic hydroxyl magnetic bead.The control to magnetic bead surfaces characteristic can be realized by the adjusting of type and additive amount to hydrophobic silane dressing agent, and above-mentioned amphiphilic hydroxyl magnetic bead has excellent hydrophily and surface reaction activity, good biocompatibility, nucleic acid can be separated, or it is coupled with bioactive substances such as albumen, antibody, to realize the identification of bioactive substance, application value with higher.
Description
Technical field
The present invention relates to field of material technology, in particular to amphiphilic hydroxyl magnetic bead and its preparation method and application.
Background technique
Magnetic bead is a kind of novel functional material, and it is a series of solely to have magnetic conductance tropism, high-specific surface area, bio-compatibility etc.
Special and superior physicochemical property, can effectively shorten experimental period, be a kind of novel efficient reagent.Include inside magnetic bead
One magnetic core, common magnetic core are Fe3O4With γ-Fe2O3, can assemble rapidly in the presence of magnetic field, leaving magnetic field can be uniform
Dispersion.Li Yadongs et al. etc. prepare Fe using solvent-thermal method3O4Magnetic kernel using ferric trichloride, ethylene glycol, sodium acetate and gathers
Ethylene glycol is raw material, in 200 DEG C of high-temperature high-voltage reaction 8h, 200~800nm magnetic kernel derived above.But magnetic made from this method
Existing Van der Waals force and polarity will lead to magnetic bead and largely reunite between pearl, while magnetic bead there is also stability difference and is easy
The disadvantages of oxidation.Although magnetic bead is modified or is wrapped up by silica, to avoid magnetic bead oxidation and keep magnetic property,
It improves the stability of magnetic bead and increases its hydrophily, and hydrophobization is carried out to water-soluble magnetic bead by surfactant (such as oleic acid)
Modification, or the hydrophobicity that polymer composite microsphere improves magnetic bead is obtained by monomer polymerization (such as styrene), it can be to a certain degree
The upper improvement above problem.But hydrophobization modification is carried out to magnetic bead with oleic acid and styrene, it is difficult to be precisely controlled hydrophobicity power
With hydrophobicity density, and then be difficult to control magnetic bead surface characteristic.
Summary of the invention
Based on this, it is necessary to provide a kind of amphiphilic hydroxyl magnetic bead and its preparation method and application that surface characteristic is controllable.
A kind of preparation method of amphiphilic hydroxyl magnetic bead, comprising the following steps: by Fe3O4Magnetic particles 0.5g~5g, hydrophily
Hydride modified dose of 1mL~20mL, hydrophobic silane dressing agent 0mL~10mL, catalyst 5mL~20mL and solvent 400mL~
2500mL mixing, reacts at 25~80 DEG C；Black precipitate substance is collected after reaction, and washing is drying to obtain described amphiphilic
Hydroxyl magnetic bead；
The hydrophilic silane dressing agent be withStructure silane, wherein R1、R2、R3And R4In at least
One is alkoxy；
The hydrophobic silane dressing agent be withThe silane of structure, wherein the R5、R6、R7And R8In extremely
Rare one is alkoxy, and at least there are one be C1-C18 alkyl, vinyl, phenyl or epoxy group.
And the hydrophily of the hydrophilic silane dressing agent is greater than the hydrophily of the hydrophobic silane dressing agent.
The preparation method of above-mentioned amphiphilic hydroxyl magnetic bead is with Fe3O4Magnetic particles, hydrophilic silane dressing agent, hydrophobic silane
Dressing agent, catalysts and solvents are raw material, by using hydride modified dose to Fe3O4Magnetic bead is modified, so that being obtained
Controllable amphiphilic silicone hydroxyl magnetic bead surfaces contain a large amount of silicone hydroxyl groups, have excellent hydrophily and surface reaction activity,
Can also carry out functional grafting, good biocompatibility can separate nucleic acid, or with the bioactive substances such as albumen, antibody
Coupling, thus realize the identification of bioactive substance, application value with higher.
Further, since hydrophilic silane dressing agent and hydrophobic silane dressing agent are the silane containing alkoxy, structure phase
Seemingly, energy hydrolytic crosslinking generates silica, passes through the i.e. adjustable parents of the type for adjusting hydrophobic silane dressing agent and additive amount
Property hydroxyl magnetic bead hydrophily and hydrophobicity, moreover it is possible to selectively on amphiphilic hydroxyl magnetic bead introduce hydrophobic group or other
Functional group, to realize the control to magnetic bead surfaces characteristic.And it can also be adjusted by adjusting hydrophobic silane dressing agent double
The surface parameters such as specific surface area, Kong Rong and the silicone hydroxyl density of parent's property hydroxyl magnetic bead, and then magnetic bead surfaces characteristic is carried out rationally
Adjustment, realizes different demands.
Furthermore this method raw material sources are extensive, low in cost, and preparation process is simple, and reaction condition is mild, without adding
Pressure, low energy consumption, without special instruments and equipment, batch production easy to accomplish, and difference between batch is small.And the above method can be prepared into
To the amphiphilic hydroxyl magnetic bead of nanoscale, and particle diameter distribution is uniform, can reduce and treat the biology that detection substance is especially such as cell
The damage of active material is small, effectively improves separative efficiency.
In one embodiment, the R in the hydrophilic silane dressing agent1、R2、R3And R4In be alkoxy.
In one embodiment, the Fe3O4Magnetic particles be 0.6g~3g, the hydrophilic silane dressing agent be 5mL~
15mL, the hydrophobic silane dressing agent are 0.1mL~3mL, and the catalyst is 5mL~20mL and the solvent is 200mL
~2500mL.
In one embodiment, the hydrophilic silane dressing agent is selected from: tetramethoxy-silicane, tetraethoxysilane,
One of tetrapropoxysilane and triethoxysilane are a variety of.
In one embodiment, the hydrophobic silane dressing agent is selected from: methyltrimethoxysilane, three ethoxy of methyl
Base silane, dimethyl diethoxysilane, trimethylethoxysilane, propyl trimethoxy silicane, octyl trimethoxy silane,
Octadecyl trimethoxysilane, methyl vinyl diethoxysilane, vinyltriethoxysilane, phenyl trimethoxy silicon
Alkane, dimethoxydiphenylsilane, 3- glycidyloxypropyl trimethoxy silane, diethoxymethyl phenyl silane and
One of dimethoxymethylphenylsilane is a variety of.
In one embodiment, the volume ratio of the hydrophilic silane dressing agent and hydrophobic silane dressing agent be (2~
20):1。
In one embodiment, the catalyst is acidic catalyst or basic catalyst；The acidic catalyst choosing
From one of acetic acid, hydrochloric acid and sulfuric acid or a variety of；The basic catalyst is selected from one of ammonium hydroxide and sodium hydroxide or more
Kind.
In one embodiment, the solvent is the mixed liquor of water and alcohol.
In one embodiment, the volume ratio of the water and alcohol is (2~6): 1.
The preparation method of above-mentioned amphiphilic hydroxyl magnetic bead, comprising the following steps:
By the Fe3O4Magnetic particles, hydrophilic silane dressing agent, hydrophobic silane dressing agent, catalysts and solvents mixing,
It is reacted at 25~80 DEG C；Black precipitate substance is collected after reaction, and washing is drying to obtain the amphiphilic hydroxyl magnetic bead.
In one embodiment, by the Fe3O4Magnetic particles, hydrophilic silane dressing agent, hydrophobic silane dressing agent,
After catalysts and solvents mixing, with 200~800 revs/min of 6~96h of speed responsing at 25~80 DEG C.
In one embodiment, the concrete operations of black precipitate substance are collected are as follows:
After reaction solution strong magnets are attracted to supernatant be it is colourless, discard supernatant to get black precipitate substance.
The amphiphilic hydroxyl magnetic bead that the preparation method of above-mentioned amphiphilic hydroxyl magnetic bead is prepared.
Application of the above-mentioned amphiphilic hydroxyl magnetic bead in biological active matter quality detection.
Above-mentioned controllable amphiphilic silicone hydroxyl magnetic bead surfaces contain a large amount of silicone hydroxyl groups, have excellent hydrophily and surface
Reactivity can also carry out functional grafting, and good biocompatibility can separate nucleic acid, or biological with albumen, antibody etc.
Active material coupling, to realize the identification of bioactive substance.
Application of the above-mentioned amphiphilic hydroxyl magnetic bead in preparation oil removing material.
Above-mentioned amphiphilic hydroxyl magnetic bead is easier to realize the adjusting of surface characteristic, moreover it is possible to be selectively introduced dredging for various carbochains
Aqueous group is advantageously used for the enrichment of lyophobic dust, can be used for detecting micro hydrophobic substance in water, or be used to prepare and remove
Light wood material.
Detailed description of the invention
Fig. 1 is the transmission electron microscope and grain size distribution of the controllable amphiphilic silicone hydroxyl magnetic bead of embodiment 1-4；
Fig. 2 is the specific surface area and Kong Rongtu of the controllable amphiphilic silicone hydroxyl magnetic bead of embodiment 1- embodiment 4.
Specific embodiment
To facilitate the understanding of the present invention, below will to invention is more fully described, and give it is of the invention compared with
Good embodiment.But the invention can be realized in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
Being exemplified below specific embodiment, the present invention will be described.
It should be noted that following Fe3O4@SiO2-OH/CX%, wherein X% refers to that hydrophobic silane dressing agent accounts in raw material
Hydride modified dose of percent by volume, wherein hydride modified dose refers to hydrophobic silane dressing agent and hydrophilic silane dressing agent
Summation.
Embodiment 1
Controllable amphiphilic silicone hydroxyl magnetic bead Fe3O4@SiO2-OH/C0%Preparation method
1g Fe is weighed first3O4Magnetic particles (making by oneself according to Li Yadong's method) are put into 2000mL three-necked flask, are measured
1000mL ethyl alcohol, 250mL water, 10mL ammonium hydroxide, 8mL tetraethoxysilane and 0mL methyltrimethoxysilane are added to three mouthfuls of burnings
In bottle, ultrasonic 30min is uniformly dispersed.Three-necked flask is placed in 25 DEG C of water-baths and is heated, is stirred with 500 revs/min of rate machinery
It mixes for 24 hours, after reaction, is down to room temperature, obtain black magnetic bead aaerosol solution.After above-mentioned reaction solution strong magnets are attracted extremely
Supernatant be it is colourless, discard supernatant, black precipitate water and alcohol mixeding liquid clean up repeatedly, and sample is put into drying box
70 DEG C of dryings obtain final sample controllably amphiphilic silicone hydroxyl magnetic bead Fe for 24 hours3O4@SiO2-OH/C0%.To controllable amphiphilic silicon hydroxyl
Base magnetic bead carries out transmission electron microscope, specific surface area and hole and holds test.
As shown in Figure 1, magnetic bead is evenly distributed under transmission electron microscope, magnetic bead surfaces are enclosed with one layer of thin silicon dioxide layer,
Rough surface contains a large amount of silicone hydroxyls.Partial size is carried out to the picture of transmission electron microscope to count to obtain grain size distribution, most of magnetic bead
Partial size between 330~480nm, median 415nm, partial size is in normal distribution, and monodispersity is good.As shown in Fig. 2,
The specific surface area of magnetic bead is 52.58m2/ g, Kong Rong are 12.08cm3/ g, specific surface area and Kong Rong are bigger.The silicon of magnetic bead surfaces
Hydroxy number is more, has hydrophily.By being analyzed above it is found that 1 method of embodiment can prepare controllable amphiphilic silicone hydroxyl magnetic
Pearl Fe3O4@SiO2-OH/C0%。
Embodiment 2
Controllable amphiphilic silicone hydroxyl magnetic bead Fe3O4@SiO2-OH/C5%Preparation method
1g Fe is weighed first3O4Magnetic particles (making by oneself according to Li Yadong's method) are put into 2000mL three-necked flask, are measured
1000mL ethyl alcohol, 250mL water, 10mL ammonium hydroxide, 7.6mL tetraethoxysilane and 0.4mL methyltrimethoxysilane are added to three
In mouth flask, ultrasonic 30min is uniformly dispersed.Three-necked flask is placed in 25 DEG C of water-baths and is heated, with 500 revs/min of rate machine
Tool stirs for 24 hours, after reaction, is down to room temperature, obtains black magnetic bead aaerosol solution.Above-mentioned reaction solution strong magnets are attracted
Afterwards to supernatant be it is colourless, discard supernatant, black precipitate water and alcohol mixeding liquid clean up repeatedly, and sample is put into drying
70 DEG C of dryings obtain final sample controllably amphiphilic silicone hydroxyl magnetic bead Fe for 24 hours in case3O4@SiO2-OH/C5%.To controllable amphiphilic
Silicone hydroxyl magnetic bead carries out transmission electron microscope, specific surface area and hole and holds test.
As shown in Figure 1, magnetic bead is evenly distributed under transmission electron microscope, magnetic bead surfaces are enclosed with one layer of thin silicon dioxide layer,
Rough surface contains a large amount of silicone hydroxyls.Partial size is carried out to the picture of transmission electron microscope to count to obtain grain size distribution, most of magnetic bead
Partial size between 340~480nm, median 410nm, partial size is in normal distribution, and monodispersity is good.Through 5% dredge
After the processing of aqueous silane dressing agent, magnetic bead partial hydrophilicity surface conversion both has the wetting in water system at hydrophobic surface
Property and suspension, and can avoid in organic system particle and assemble and be sharply thickened phenomenon, successfully reach amphiphilic.Moreover, with
Magnetic bead prepared by embodiment 2 compares, specific surface area (49.37m2/ g) and Kong Rong (11.34cm3/ g) all become smaller (Fig. 2), magnetic bead table
The silicone hydroxyl density in face becomes smaller, and magnetic bead surfaces can reduce, and reduces reunion risk.The 2 method energy of embodiment known to analyzing above
It is enough to prepare controllable amphiphilic silicone hydroxyl magnetic bead Fe3O4@SiO2-OH/C5%。
Embodiment 3
Controllable amphiphilic silicone hydroxyl magnetic bead Fe3O4@SiO2-OH/C10%Preparation method
1g Fe is weighed first3O4Magnetic particles (making by oneself according to Li Yadong's method) are put into 2000mL three-necked flask, are measured
1000mL ethyl alcohol, 250mL water, 10mL ammonium hydroxide, 7.2mL tetraethoxysilane and 0.8mL methyltrimethoxysilane are added to three
In mouth flask, ultrasonic 30min is uniformly dispersed.Three-necked flask is placed in 25 DEG C of water-baths and is heated, with 500 revs/min of rate machine
Tool stirs for 24 hours, after reaction, is down to room temperature, obtains black magnetic bead aaerosol solution.Above-mentioned reaction solution strong magnets are attracted
Afterwards to supernatant be it is colourless, discard supernatant, black precipitate water and alcohol mixeding liquid clean up repeatedly, and sample is put into drying
70 DEG C of dryings obtain final sample controllably amphiphilic silicone hydroxyl magnetic bead Fe for 24 hours in case3O4@SiO2-OH/C10%.To controllable amphiphilic
Silicone hydroxyl magnetic bead carries out transmission electron microscope, specific surface area and hole and holds test.
As shown in Figure 1, magnetic bead is evenly distributed under transmission electron microscope, magnetic bead surfaces are enclosed with one layer of thin silicon dioxide layer,
Rough surface contains a large amount of silicone hydroxyls.Partial size is carried out to the picture of transmission electron microscope to count to obtain grain size distribution, most of magnetic bead
Partial size between 340~460nm, median 410nm, partial size is in normal distribution, and monodispersity is good.Through 10% dredge
After the processing of aqueous silane dressing agent, magnetic bead partial hydrophilicity surface conversion both has the wetting in water system at hydrophobic surface
Property and suspension, and can avoid in organic system particle and assemble and be sharply thickened phenomenon, successfully reach amphiphilic.Moreover, with
Magnetic bead prepared by comparative example 1 and example 2 compares, specific surface area (46.76m2/ g) and Kong Rong (10.74cm3/ g) all successively become smaller (figure
2), can be by various parameters controllable adjustment surface property, therefore, the silicone hydroxyl density of magnetic bead surfaces becomes smaller, magnetic bead surfaces energy
It reduces, reduces reunion risk.By being analyzed above it is found that the method for embodiment 3 can prepare controllable amphiphilic silicone hydroxyl magnetic bead
Fe3O4@SiO2-OH/C10%。
Embodiment 4
Controllable amphiphilic silicone hydroxyl magnetic bead Fe3O4@SiO2-OH/C15%Preparation method
1g Fe is weighed first3O4Magnetic particles (making by oneself according to Li Yadong's method) are put into 2000mL three-necked flask, are measured
1000mL ethyl alcohol, 250mL water, 10mL ammonium hydroxide, 6.8mL tetraethoxysilane and 1.2mL methyltrimethoxysilane are added to three
In mouth flask, ultrasonic 30min is uniformly dispersed.Three-necked flask is placed in 25 DEG C of water-baths and is heated, with 500 revs/min of rate machine
Tool stirs for 24 hours, after reaction, is down to room temperature, obtains black magnetic bead aaerosol solution.Above-mentioned reaction solution strong magnets are attracted
Afterwards to supernatant be it is colourless, discard supernatant, black precipitate water and alcohol mixeding liquid clean up repeatedly, and sample is put into drying
70 DEG C of dryings obtain final sample controllably amphiphilic silicone hydroxyl magnetic bead Fe for 24 hours in case3O4@SiO2-OH/C15%.To controllable amphiphilic
Silicone hydroxyl magnetic bead carries out transmission electron microscope, specific surface area and hole and holds test.
As shown in Figure 1, magnetic bead is evenly distributed under transmission electron microscope, magnetic bead surfaces are enclosed with one layer of thin silicon dioxide layer,
Rough surface contains a large amount of silicone hydroxyls.Partial size is carried out to the picture of transmission electron microscope to count to obtain grain size distribution, most of magnetic bead
Partial size between 340~440nm, median 390nm, partial size is in normal distribution, and monodispersity is good.Through 15% dredge
After the processing of aqueous silane dressing agent, magnetic bead partial hydrophilicity surface conversion both has the wetting in water system at hydrophobic surface
Property and suspension, and can avoid in organic system particle and assemble and be sharply thickened phenomenon, successfully reach amphiphilic.Moreover, with
Magnetic bead prepared by embodiment 1- embodiment 3 compares, specific surface area (45.73m2/ g) and Kong Rong (10.51cm3/ g) all successively become smaller
(Fig. 2), can be by various parameters controllable adjustment surface property, therefore, and the silicone hydroxyl density of magnetic bead surfaces becomes smaller, magnetic bead surfaces
It can reduce, reduce reunion risk.By being analyzed above it is found that 4 method of embodiment can prepare controllable amphiphilic silicone hydroxyl magnetic bead
Fe3O4@SiO2-OH/C15%。
As a result such as table 1 is summarized
Table 1
As it can be seen from table 1 the particle diameter distribution of above-mentioned amphiphilic silicone hydroxyl magnetic bead is uniform, pass through hydrophobic silane dressing agent
Addition the adjusting of magnetic bead surfaces characteristic can be realized.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of amphiphilic hydroxyl magnetic bead, which comprises the following steps:
By Fe3O4Magnetic particles 0.5g~5g, hydrophilic silane dressing agent 1mL~20mL, hydrophobic silane dressing agent 0mL~10mL,
Catalyst 5mL~20mL and solvent 200mL~2500mL mixing, reacts at 25~80 DEG C；It is heavy that black is collected after reaction
Starch matter, washing are drying to obtain the amphiphilic hydroxyl magnetic bead；
The hydrophilic silane dressing agent be withThe silane of structure, wherein R1、R2、R3And R4In at least one be
Alkoxy；
The hydrophobic silane dressing agent be withThe silane of structure, wherein the R5、R6、R7And R8In at least one
A is alkoxy, and at least there are one be C1-C18 alkyl, vinyl, phenyl or epoxy group；
And the hydrophily of the hydrophilic silane dressing agent is greater than the hydrophily of the hydrophobic silane dressing agent.
2. the preparation method of amphiphilic hydroxyl magnetic bead according to claim 1, which is characterized in that the hydrophilic silane is repaired
Decorations agent is selected from: one of tetramethoxy-silicane, tetraethoxysilane, tetrapropoxysilane and triethoxysilane are a variety of.
3. the preparation method of amphiphilic hydroxyl magnetic bead according to claim 1, which is characterized in that the hydrophobic silane is repaired
Decorations agent is selected from: methyltrimethoxysilane, methyltriethoxysilane, dimethyl diethoxysilane, front three base oxethyl silicon
Alkane, propyl trimethoxy silicane, octyl trimethoxy silane, octadecyl trimethoxysilane, methyl ethylene diethoxy
Silane, vinyltriethoxysilane, phenyltrimethoxysila,e, dimethoxydiphenylsilane, 3- glycidyl oxygroup
One of propyl trimethoxy silicane, diethoxymethyl phenyl silane and dimethoxymethylphenylsilane are a variety of.
4. the preparation method of amphiphilic hydroxyl magnetic bead according to claim 1-3, which is characterized in that described hydrophilic
Property hydride modified dose and hydrophobic silane dressing agent volume ratio be (2~20): 1.
5. the preparation method of amphiphilic hydroxyl magnetic bead according to claim 1-3, which is characterized in that the catalysis
Agent is acidic catalyst or basic catalyst；The acidic catalyst is selected from one of acetic acid, hydrochloric acid and sulfuric acid or a variety of；Institute
It states basic catalyst and is selected from one of ammonium hydroxide and sodium hydroxide or a variety of.
6. the preparation method of amphiphilic hydroxyl magnetic bead according to claim 1-3, which is characterized in that the solvent
For the mixed liquor of water and alcohol.
7. the preparation method of amphiphilic hydroxyl magnetic bead according to claim 6, which is characterized in that the volume of the water and alcohol
Than for (2~6): 1.
8. the amphiphilic hydroxyl magnetic that the preparation method of the described in any item amphiphilic hydroxyl magnetic beads of claim 1-7 is prepared
Pearl.
9. application of the amphiphilic hydroxyl magnetic bead according to any one of claims 8 in biological active matter quality detection.
10. application of the amphiphilic hydroxyl magnetic bead according to any one of claims 8 in preparation oil removing material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110211757A (en) * | 2019-05-24 | 2019-09-06 | 清华大学 | With amphipathic and magnetic nano particle and preparation method thereof |
| CN111579772A (en) * | 2020-05-28 | 2020-08-25 | 珠海丽珠试剂股份有限公司 | Detection reagent based on immunomagnetic bead method, preparation method thereof, kit and detection method |
| CN112213174A (en) * | 2019-07-12 | 2021-01-12 | 南京岚煜生物科技有限公司 | Method for uniformly mixing magnetic materials |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101553889A (en) * | 2006-09-05 | 2009-10-07 | 哥伦布纳米制品公司 | Magnetic particles and methods of making and using the same |
| CN101574645A (en) * | 2009-06-05 | 2009-11-11 | 中国科学院生态环境研究中心 | Magnetic nano-material extractant and preparation method thereof |
| EP2804186A1 (en) * | 2013-05-14 | 2014-11-19 | King Saud University | Coated magnetite nanoparticles, method for the preparation thereof and their use |
| CN105950132A (en) * | 2016-04-20 | 2016-09-21 | 吉林大学 | Amphiphilic silane-coated water-soluble composite nano-material and application thereof |
-
2018
- 2018-12-04 CN CN201811473412.1A patent/CN109559882A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101553889A (en) * | 2006-09-05 | 2009-10-07 | 哥伦布纳米制品公司 | Magnetic particles and methods of making and using the same |
| CN101574645A (en) * | 2009-06-05 | 2009-11-11 | 中国科学院生态环境研究中心 | Magnetic nano-material extractant and preparation method thereof |
| EP2804186A1 (en) * | 2013-05-14 | 2014-11-19 | King Saud University | Coated magnetite nanoparticles, method for the preparation thereof and their use |
| CN105950132A (en) * | 2016-04-20 | 2016-09-21 | 吉林大学 | Amphiphilic silane-coated water-soluble composite nano-material and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 林祥华: "可控双亲性硅羟基磁珠Fe3O4@SiO2的制备", 《周口师范学院学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110211757A (en) * | 2019-05-24 | 2019-09-06 | 清华大学 | With amphipathic and magnetic nano particle and preparation method thereof |
| CN112213174A (en) * | 2019-07-12 | 2021-01-12 | 南京岚煜生物科技有限公司 | Method for uniformly mixing magnetic materials |
| CN111579772A (en) * | 2020-05-28 | 2020-08-25 | 珠海丽珠试剂股份有限公司 | Detection reagent based on immunomagnetic bead method, preparation method thereof, kit and detection method |
| CN111579772B (en) * | 2020-05-28 | 2022-04-08 | 珠海丽珠试剂股份有限公司 | Detection reagent based on immunomagnetic bead method, preparation method thereof, kit and detection method |
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