CN107768061B - A kind of preparation method of packet silicon nanoscale magnetic bead - Google Patents
A kind of preparation method of packet silicon nanoscale magnetic bead Download PDFInfo
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- CN107768061B CN107768061B CN201710804936.3A CN201710804936A CN107768061B CN 107768061 B CN107768061 B CN 107768061B CN 201710804936 A CN201710804936 A CN 201710804936A CN 107768061 B CN107768061 B CN 107768061B
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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
- H01F1/0018—Diamagnetic or paramagnetic materials, i.e. materials with low susceptibility and no hysteresis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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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
Abstract
The present invention discloses a kind of preparation method of packet silicon nanoscale magnetic bead, by silicon ball solution of the preparation containing Nano particles of silicon dioxide, magnetic ball is prepared, the silicon ball solution and the magnetic ball are stirred are mixed to get the magnetic ball for being adsorbed with silicon ball, the magnetic ball for being adsorbed with silicon ball is transferred to alcohol-water system and utilizes TEOS sol-gal process, so that the silicon ball forms silicon layer on the surface of the magnetic ball, washing obtains product packet silicon nanoscale magnetic bead after Magneto separate.A kind of preparation method of packet silicon nanoscale magnetic bead of the present invention, method is simple and safe, cost of material is low, suitable for industry's enlarging production, nanoscale magnetic bead good dispersion, the magnetic responsiveness being prepared are strong, and monodispersed packet silicon nanoscale magnetic bead has broad application prospects in fields such as bio-separation, environment, catalysis, Solid Phase Extraction.
Description
Technical field
The present invention relates to the magnanimity preparation fields of magnetic nano composite microsphere, and in particular to be a kind of packet silicon nanoscale magnetic bead
Preparation method.
Background technique
Magnetic nanoparticle has skin effect, small-size effect, quantum effect and superparamagnetism, keeps it wide according to having
Application prospect, thus be concerned.The nano particle of typical superparamagnetism is mainly metal oxide, such as Fe3O4、Y-
Fe2O3、MO·Fe2O3(M Co, Cu, Mn) etc..Nanometer Fe3O4Due to preparing, simple, magnetic response ability is strong, surface is easily modified
Feature becomes the magnetic material being most widely used at present.
Magnetic nanoparticle is easily reunited and is aoxidized, seriously affect its use process because of its small size and skin effect
In stability.Although the magnetic nanoparticle after the modification such as PEG, oleic acid, PVP, stability make moderate progress, it is steady
It is qualitative to be still difficult to more than 3 months, for Submicron magnetic nano particle of the size greater than 200nm.In magnetism
Nano grain surface coats organic and inorganic materials, such as SiO2, cellulose, polystyrene, polyacrylamide derivative etc., in turn
It is to improve magnetic nanoparticle to stablize in bio-active groups such as magnetic nanoparticle surface modification grafted amino group, carboxyl, hydroxyls
The effective means of property and biocompatibility.Wherein silica has good physical and chemical stability, biocompatibility, surface
Easily modification, can be used in a variety of different environment, thus receive significant attention.
In magnetic nanoparticle surface coated silica, the method for forming the silicon substrate magnetic nano-balls of core-shell structure is main
Have: emulsion method, TEOS sol-gal process, sodium metasilicate method.These methods there is the preparation amounts of unit volume limited, technology controlling and process
Complicated, repeatability difference common drawback, therefore cause preparation cost higher, it seriously limits it and further develops and uses.Than
As conventional TEOS sol-gal process directly coats silicon layer, body using ammonia-catalyzed teos hydrolysis in alcohol-water system
Magnetic ball is easily reunited in system, and magnetic ball concentration is difficult to improve, and production cost is high.In addition, general in practical applications require preparation
Obtained nanoscale magnetic bead has the characteristics that monodispersity, size be controllable, high-intensity magnetic field responding ability, thus magnanimity prepare monodisperse,
The packet silicon magnetic ball of high-intensity magnetic field responding ability is the urgent need for realizing its industrial applications at present.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of packet silicon nanoscale magnetic bead, and method is simple and safe, cost of material
It is low, it is suitable for industry's enlarging production, nanoscale magnetic bead good dispersion, the magnetic responsiveness being prepared are strong, monodispersed packet silicon nano magnetic
Ball has broad application prospects in fields such as bio-separation, environment, catalysis, Solid Phase Extraction.
In order to achieve the above objectives, solution of the invention is:
A kind of preparation method of packet silicon nanoscale magnetic bead, comprising the following steps:
(1) ethyl orthosilicate, basic amino acid and deionized water are injected into flask, in 50-70 DEG C of stirred in water bath
8-48h obtains silicon ball solution, is stored in spare at 4 DEG C；
(2) Iron(III) chloride hexahydrate and anhydrous sodium acetate are added in stainless steel cauldron, add PEG 2000 with
And ethylene glycol as solvent and/or diglycol form reaction solution, the ferric ion concentration control in the reaction solution
System is in 0.1-0.33mol/L, and the concentration of PEG 2000 is 25mg/mL, and machinery stirs evenly, stainless steel cauldron is sealed, 190-200
DEG C reaction 4-12h；
(3) stainless steel cauldron of step (2) by reaction is taken out, room temperature is cooling, pours out reaction solution, will be generated with magnet
Magnetic ball separated from reaction solution, wash repeatedly magnetic ball respectively 3-4 times with deionized water and dehydrated alcohol, then by magnetic ball point
It dissipates and forms black magnetic fluid in deionized water, save backup；
(4) take the black magnetic fluid containing 1-20g magnetic ball in flask, the upper layer that Magneto separate removes in flask is clear
The hydrochloric acid solution that 100-500mL concentration is 0.1-0.5mol/L, mechanical stirring 5-30min is added in liquid；
(5) Magneto separate removes the supernatant liquor in the flask after hydrochloric acid solution is added in step (4), adds 150-
The silicon ball solution and 100-350mL deionized water, mechanical stirring 3-12h, Magneto separate of 350mL step (1) preparation obtain
Adsorption has the magnetic ball of silicon ball spare；
(6) the magnetic ball that adsorption obtained in step (5) has silicon ball is re-dispersed into 300-500mL volume fraction is
In the ethyl alcohol of 80-90%, 10-25mL concentrated ammonia liquor and 1-15mL ethyl orthosilicate is added, 0.5-5h is stirred at room temperature；Magneto separate obtains
It is coated with the magnetic ball of silicon layer, is washed to neutrality with deionized water and dehydrated alcohol to get the packet silicon nanoscale magnetic bead.
In step (1), the dosage molar ratio of the ethyl orthosilicate, basic amino acid and deionized water is 1-5: 0.02:
162。
In step (1), the basic amino acid is arginine or lysine.
In step (1), the preparation of the silicon ball solution needs 50-70 DEG C of water bath with thermostatic control, and system pH maintains 9-11, obtains
The size of silicon dioxide microsphere is in 12-25nm.
In step (2), the dosage molar ratio of the Iron(III) chloride hexahydrate and the anhydrous sodium acetate is 1: 3-10.
In step (2), when the solvent is the mixed alcohol of ethylene glycol and diglycol, ethylene glycol and a contracting diethyl two
The volumetric usage ratio of alcohol is 1-2: 2-1.Change ethylene glycol and diglycol in reaction system with when source of iron content can
To regulate and control the size for the magnetic ball that step (3) obtains between 100-600nm.
In step (4), the purpose that the hydrochloric acid is added is due to the reaction system that silicon ball is adsorbed under stiring in step (5)
PH need to control between 4-6.5, prefabricated silicon ball is adsorbed on magnetic ball surface, increases magnetic ball in dispersing agent (water, ethyl alcohol)
Electrostatic repulsion, and then be easy to be adsorbed with silicon ball magnetic ball surface carry out silicon layer growth.
In step (6), the silicon of the adjustable magnetic ball surface for being adsorbed with silicon ball of the change of the additional amount of the ethyl orthosilicate
Layer growth thickness.
A kind of preparation method of packet silicon nanoscale magnetic bead of the present invention, it is molten by silicon ball of the preparation containing Nano particles of silicon dioxide
Liquid prepares magnetic ball (main component Fe3O4), the silicon ball solution and the magnetic ball is stirred to be mixed to get and is adsorbed with silicon
The magnetic ball for being adsorbed with silicon ball is transferred to alcohol-water system and utilizes TEOS sol-gal process, so that the silicon by the magnetic ball of ball
The characteristics of ball forms silicon layer on the surface of the magnetic ball, washs after Magneto separate and obtains product packet silicon nanoscale magnetic bead, the preparation method
Be, due to silicon ball solution and magnetic ball be stirred mixing before be added hydrochloric acid regulation system pH, increase magnetic ball point
Electrostatic repulsion in powder, and then be easy to carry out the growth of silicon layer in the magnetic ball surface for being adsorbed with small silicon ball.
After adopting the above technical scheme, a kind of preparation method of packet silicon nanoscale magnetic bead of the present invention, overcomes in alcohol-water system
In be introduced directly into the ethyl orthosilicate cladding silicon layer problem that causes magnetic ball easy to reunite, thus silicon can will be adsorbed in reaction system
The concentration of the magnetic ball of ball is increased to 10g/L or more from 1g/L, to reach the nucleocapsid that magnanimity prepares monodisperse, high-intensity magnetic field responsiveness
The purpose of the silicon substrate magnetic nanoparticle of structure.The preparation method raw material is easy to get, simple process, is easy to amplify production, thus has
Have broad application prospects.
Specific embodiment
In order to further explain the technical solution of the present invention, being explained in detail below by specific embodiment the present invention
It states.
Embodiment one
A kind of preparation method of packet silicon nanoscale magnetic bead, comprising the following steps:
(1) 1.197g arginine is dissolved in the three-necked flask equipped with 1000mL deionized water, is stirred in 50 DEG C of water-baths
It mixes, then 71.5g ethyl orthosilicate is added into three-necked flask, continue stirring for 24 hours, obtain silicon ball solution, be stored in 4 DEG C of refrigerators
It is spare；
(2) 32.4g Iron(III) chloride hexahydrate, 98.44g anhydrous sodium acetate are added in stainless steel cauldron, are added
30g PEG 2000 and 1200mL diglycol, form reaction solution, and the ferric ion concentration in reaction solution is
The concentration of 0.1mol/L, PEG 2000 is 25mg/mL, and machinery stirs evenly, stainless steel cauldron is sealed, 190 DEG C of reaction 4h；
(3) stainless steel cauldron of step (2) by reaction is taken out, room temperature is cooling, pours out reaction solution, will be generated with magnet
Magnetic ball separated from reaction solution, washed repeatedly respectively magnetic ball 3 times with deionized water and dehydrated alcohol, then magnetic ball is dispersed
Black magnetic fluid is formed in deionized water, is saved backup；
(4) take the black magnetic fluid containing 5g magnetic ball in three-necked flask, the upper layer that Magneto separate removes in three-necked flask is clear
The hydrochloric acid solution that 500mL concentration is 0.5mol/L, mechanical stirring 5min is added in liquid；
(5) Magneto separate removes the supernatant liquor in the three-necked flask after hydrochloric acid solution is added in step (4), adds
The silicon ball solution and 350mL deionized water of 350mL step (1) preparation, mechanical stirring 3h, Magneto separate, which obtains adsorption, silicon
The magnetic ball of ball is spare；
(6) the magnetic ball that adsorption obtained in step (5) has silicon ball is re-dispersed into 500mL volume fraction is 90%
Ethyl alcohol in, 25mL concentrated ammonia liquor and 15mL ethyl orthosilicate is added, 5h is stirred at room temperature；Magneto separate obtains the magnetic for being coated with silicon layer
Ball, with deionized water and dehydrated alcohol wash to neutrality to get size 100nm packet silicon nanoscale magnetic bead.
Embodiment two
A kind of preparation method of packet silicon nanoscale magnetic bead, comprising the following steps:
(1) 1.197g arginine is dissolved in the three-necked flask equipped with 1000mL deionized water, is stirred in 70 DEG C of water-baths
It mixes, then 71.5g ethyl orthosilicate is added into three-necked flask, continue to stir 8h, obtain silicon ball solution, be stored in 4 DEG C of refrigerators
It is spare；
(2) 108.2g Iron(III) chloride hexahydrate, 98.44g anhydrous sodium acetate are added in stainless steel cauldron, are added
30g PEG 2000 and 1200mL diglycol, form reaction solution, and the ferric ion concentration in reaction solution is
The concentration of 0.33mol/L, PEG 2000 is 25mg/mL, and machinery stirs evenly, stainless steel cauldron is sealed, 190 DEG C of reaction 12h；
(3) stainless steel cauldron of step (2) by reaction is taken out, room temperature is cooling, pours out reaction solution, will be generated with magnet
Magnetic ball separated from reaction solution, washed repeatedly respectively magnetic ball 3 times with deionized water and dehydrated alcohol, then magnetic ball is dispersed
Black magnetic fluid is formed in deionized water, is saved backup；
(4) take the black magnetic fluid containing 1g magnetic ball in three-necked flask, the upper layer that Magneto separate removes in three-necked flask is clear
The hydrochloric acid solution that 100mL concentration is 0.1mol/L, mechanical stirring 5min is added in liquid；
(5) Magneto separate removes the supernatant liquor in the three-necked flask after hydrochloric acid solution is added in step (4), adds
The silicon ball solution and 350mL deionized water of 150mL step (1) preparation, mechanical stirring 12h, Magneto separate, which obtains adsorption, to be had
The magnetic ball of silicon ball is spare；
(6) the magnetic ball that adsorption obtained in step (5) has silicon ball is re-dispersed into 500mL volume fraction is 80%
Ethyl alcohol in, 10mL concentrated ammonia liquor and 1mL ethyl orthosilicate is added, 0.5h is stirred at room temperature；Magneto separate obtains the magnetic for being coated with silicon layer
Ball, with deionized water and dehydrated alcohol wash to neutrality to get size 105nm packet silicon nanoscale magnetic bead.
Embodiment three
A kind of preparation method of packet silicon nanoscale magnetic bead, comprising the following steps:
(1) 1.197g arginine is dissolved in the three-necked flask equipped with 1000mL deionized water, is stirred in 70 DEG C of water-baths
It mixes, then 357.5g ethyl orthosilicate is added into three-necked flask, continue to stir 48h, obtain silicon ball solution, be stored in 4 DEG C of refrigerators
In it is spare；
(2) 108.12g Iron(III) chloride hexahydrate, 98.44g anhydrous sodium acetate are added in stainless steel cauldron, then plus
Enter 30g PEG 2000,400mL ethylene glycol and 800mL diglycol, form reaction solution, the ferric iron in reaction solution from
Sub- concentration is 0.33mol/L, and the concentration of PEG 2000 is 25mg/mL, and machinery, which stirs evenly, seals stainless steel cauldron, and 190 DEG C anti-
Answer 12h；
(3) stainless steel cauldron of step (2) by reaction is taken out, room temperature is cooling, pours out reaction solution, will be generated with magnet
Magnetic ball separated from reaction solution, washed repeatedly respectively magnetic ball 3 times with deionized water and dehydrated alcohol, then magnetic ball is dispersed
Black magnetic fluid is formed in deionized water, is saved backup；
(4) take the black magnetic fluid containing 1g magnetic ball in three-necked flask, the upper layer that Magneto separate removes in three-necked flask is clear
The hydrochloric acid solution that 100mL concentration is 0.1mol/L, mechanical stirring 30min is added in liquid；
(5) Magneto separate removes the supernatant liquor in the three-necked flask after hydrochloric acid solution is added in step (4), adds
The silicon ball solution and 350mL deionized water of 150mL step (1) preparation, mechanical stirring 12h, Magneto separate, which obtains adsorption, to be had
The magnetic ball of silicon ball is spare；
(6) the magnetic ball that adsorption obtained in step (5) has silicon ball is re-dispersed into 500mL volume fraction is 90%
Ethyl alcohol in, 25mL concentrated ammonia liquor and 15mL ethyl orthosilicate is added, 5h is stirred at room temperature；Magneto separate obtains the magnetic for being coated with silicon layer
Ball, with deionized water and dehydrated alcohol wash to neutrality to get size 210nm packet silicon nanoscale magnetic bead.
Example IV
A kind of preparation method of packet silicon nanoscale magnetic bead, comprising the following steps:
(1) 1.197g arginine is dissolved in the three-necked flask equipped with 1000mL deionized water, is stirred in 60 DEG C of water-baths
It mixes, then 71.5g ethyl orthosilicate is added into three-necked flask, continue stirring for 24 hours, obtain silicon ball solution, be stored in 4 DEG C of refrigerators
It is spare；
(2) 108.12g Iron(III) chloride hexahydrate, 98.44g anhydrous sodium acetate are added in stainless steel cauldron, then plus
Enter 30g PEG 2000,600mL ethylene glycol and 600mL diglycol, form reaction solution, the ferric iron in reaction solution from
Sub- concentration is 0.33mol/L, and the concentration of PEG 2000 is 25mg/mL, and machinery, which stirs evenly, seals stainless steel cauldron, and 200 DEG C anti-
Answer 12h；
(3) stainless steel cauldron of step (2) by reaction is taken out, room temperature is cooling, pours out reaction solution, will be generated with magnet
Magnetic ball separated from reaction solution, washed repeatedly respectively magnetic ball 3 times with deionized water and dehydrated alcohol, then magnetic ball is dispersed
Black magnetic fluid is formed in deionized water, is saved backup；
(4) take the black magnetic fluid containing 5g magnetic ball in three-necked flask, the upper layer that Magneto separate removes in three-necked flask is clear
The hydrochloric acid solution that 500mL concentration is 0.5mol/L, mechanical stirring 5min is added in liquid；
(5) Magneto separate removes the supernatant liquor in the three-necked flask after hydrochloric acid solution is added in step (4), adds
The silicon ball solution and 350mL deionized water of 350mL step (1) preparation, mechanical stirring 3h, Magneto separate, which obtains adsorption, silicon
The magnetic ball of ball is spare；
(6) the magnetic ball that adsorption obtained in step (5) has silicon ball is re-dispersed into 500mL volume fraction is 90%
Ethyl alcohol in, 25mL concentrated ammonia liquor and 15mL ethyl orthosilicate is added, 5h is stirred at room temperature；Magneto separate obtains the magnetic for being coated with silicon layer
Ball, with deionized water and dehydrated alcohol wash to neutrality to get size 315nm packet silicon nanoscale magnetic bead.
Embodiment five
A kind of preparation method of packet silicon nanoscale magnetic bead, comprising the following steps:
(1) 1.197g arginine is dissolved in the three-necked flask equipped with 1000mL deionized water, is stirred in 50 DEG C of water-baths
It mixes, then 71.5g ethyl orthosilicate is added into three-necked flask, continue stirring for 24 hours, obtain silicon ball solution, be stored in 4 DEG C of refrigerators
It is spare；
(2) 108.12g Iron(III) chloride hexahydrate, 98.44g anhydrous sodium acetate are added in stainless steel cauldron, then plus
Enter 30g PEG 2000,800mL ethylene glycol and 400mL diglycol, form reaction solution, the ferric iron in reaction solution from
Sub- concentration is 0.33mol/L, and the concentration of PEG 2000 is 25mg/mL, and machinery stirs evenly, stainless steel cauldron is sealed, and 200 DEG C anti-
Answer 12h；
(3) stainless steel cauldron of step (2) by reaction is taken out, room temperature is cooling, pours out reaction solution, will be generated with magnet
Magnetic ball separated from reaction solution, washed repeatedly respectively magnetic ball 3 times with deionized water and dehydrated alcohol, then magnetic ball is dispersed
Black magnetic fluid is formed in deionized water, is saved backup；
(4) take the black magnetic fluid containing 5g magnetic ball in three-necked flask, the upper layer that Magneto separate removes in three-necked flask is clear
The hydrochloric acid solution that 500mL concentration is 0.1mol/L, mechanical stirring 30min is added in liquid；
(5) Magneto separate removes the supernatant liquor in the three-necked flask after hydrochloric acid solution is added in step (4), adds
The silicon ball solution and 200mL deionized water of 150mL step (1) preparation, mechanical stirring 12h, Magneto separate, which obtains adsorption, to be had
The magnetic ball of silicon ball is spare；
(6) the magnetic ball that adsorption obtained in step (5) has silicon ball is re-dispersed into 300mL volume fraction is 80%
Ethyl alcohol in, 20mL concentrated ammonia liquor and 1mL ethyl orthosilicate is added, 0.5h is stirred at room temperature；Magneto separate obtains the magnetic for being coated with silicon layer
Ball, with deionized water and dehydrated alcohol wash to neutrality to get size 420nm packet silicon nanoscale magnetic bead.
Above-described embodiment and non-limiting product form and style of the invention, the ordinary skill people of any technical field
The appropriate changes or modifications that member does it, all should be regarded as not departing from patent category of the invention.
Claims (5)
1. a kind of preparation method of packet silicon nanoscale magnetic bead, it is characterised in that: the following steps are included:
(1) ethyl orthosilicate, basic amino acid and deionized water are injected into flask, in 50-70 DEG C of stirred in water bath 8-
48h obtains silicon ball solution, is stored in spare at 4 DEG C；
(2) Iron(III) chloride hexahydrate and anhydrous sodium acetate are added in stainless steel cauldron, add PEG2000 and conduct
The ethylene glycol and/or diglycol of solvent form reaction solution, and the ferric ion concentration control in the reaction solution exists
The concentration of 0.1-0.33mol/L, PEG2000 are 25mg/mL, and machinery stirs evenly, stainless steel cauldron is sealed, and 190-200 DEG C anti-
Answer 4-12h；
(3) stainless steel cauldron of step (2) by reaction is taken out, room temperature is cooling, reaction solution is poured out, with magnet by the magnetic of generation
Ball is separated from reaction solution, washes repeatedly magnetic ball respectively 3-4 times with deionized water and dehydrated alcohol, then magnetic ball is dispersed in
Black magnetic fluid is formed in deionized water, is saved backup；
(4) take the black magnetic fluid containing 1-20g magnetic ball in flask, Magneto separate removes the supernatant liquor in flask, adds
Enter the hydrochloric acid solution that 100-500mL concentration is 0.1-0.5mol/L, mechanical stirring 5-30min；
(5) Magneto separate removes the supernatant liquor in the flask after hydrochloric acid solution is added in step (4), adds 150-350mL step
Suddenly the silicon ball solution and 100-350mL deionized water of (1) preparation, so that the pH value of reaction system is 4~6.5, it is mechanical
3-12h is stirred, Magneto separate, which obtains adsorption, has the magnetic ball of silicon ball spare；
(6) the magnetic ball that adsorption obtained in step (5) has silicon ball is re-dispersed into 300-500mL volume fraction is 80-
In 90% ethyl alcohol, 10-25mL concentrated ammonia liquor and 1-15mL ethyl orthosilicate is added, 0.5-5h is stirred at room temperature；Magneto separate is wrapped
It is covered with the magnetic ball of silicon layer, is washed to neutrality with deionized water and dehydrated alcohol to get the packet silicon nanoscale magnetic bead.
2. a kind of preparation method of packet silicon nanoscale magnetic bead according to claim 1, it is characterised in that: described in step (1)
The dosage molar ratio of ethyl orthosilicate, basic amino acid and deionized water is 1-5:0.02:162.
3. a kind of preparation method of packet silicon nanoscale magnetic bead according to claim 1, it is characterised in that: described in step (1)
Basic amino acid is arginine or lysine.
4. a kind of preparation method of packet silicon nanoscale magnetic bead according to claim 1, it is characterised in that: described in step (2)
The dosage molar ratio of Iron(III) chloride hexahydrate and the anhydrous sodium acetate is 1:3-10.
5. a kind of preparation method of packet silicon nanoscale magnetic bead according to claim 1, it is characterised in that: described in step (2)
When solvent is the mixed alcohol of ethylene glycol and diglycol, the volumetric usage ratio of the ethylene glycol and the diglycol
For 1-2:2-1.
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| CN110732296B (en) * | 2018-07-18 | 2021-09-03 | 苏州为度生物技术有限公司 | Preparation method of magnetic microspheres with fluffy shell layers |
| CN109554012A (en) * | 2018-12-06 | 2019-04-02 | 武汉大学 | A kind of preparation method of bionic function gradient coating |
| CN114213562A (en) * | 2021-12-13 | 2022-03-22 | 南京工业大学 | Preparation method of magnetic polystyrene microspheres with different particle sizes |
| CN114920250A (en) * | 2022-04-12 | 2022-08-19 | 苏州星谱生物科技有限公司 | Preparation method of echinoid magnetic beads and application of echinoid magnetic beads in nucleic acid extraction |
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