CN105754021B - A kind of grain magnetic polymer microsphere preparation method - Google Patents
A kind of grain magnetic polymer microsphere preparation method Download PDFInfo
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- CN105754021B CN105754021B CN201610329610.5A CN201610329610A CN105754021B CN 105754021 B CN105754021 B CN 105754021B CN 201610329610 A CN201610329610 A CN 201610329610A CN 105754021 B CN105754021 B CN 105754021B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/34—Monomers containing two or more unsaturated aliphatic radicals
- C08F212/36—Divinylbenzene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of grain magnetic polymer microsphere preparation method.Including step：Prepare iron oleate, polymer seeds suspension, prepare iron oleate and monomer suspension, prepare initiator suspension, then, at the polymerization temperature, iron oleate monomer suspension and initiator suspension, which are added in seed suspension liquid, makes seed growth, stops adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, heat up polymerisation for the first time, continue to react, you can obtain iron oleate polymer composite microsphere.The uniform particle diameter of the magnetic polymer microsphere prepared using this method, grain diameter is controllable, magnetic is strong.
Description
Technical field
The present invention relates to a kind of grain magnetic polymer microsphere preparation method, belong to technical field of polymer materials.
Background technology
Magnetic microsphere has a wide range of applications in bio-separation engineering and biomedical engineering, especially nucleic acid extraction,
Cell separation, immobilised enzymes, immune detection, targeted drug, protein and enzyme isolate and purify etc. have in field it is tempting should
Use prospect.
The method of prior art synthesizing magnetic polymer microballoon mainly has investment, monomer polymerization method and interfacial deposition method
Deng.
United States Patent (USP) (US 4,339,337 and US 4,358,388) discloses suspension polymerization and micro-suspension polymerization, i.e.,
The oil phase of the ferric oxide particles of magnetic four, lipophile vinyl monomer and the oil-soluble initiator composition of oleophylicization processing is dispersed in water
Xiang Zhong, in the presence of mechanical agitation and stabilizer, oil phase is dispersed in aqueous phase in drop state, adds thermal-initiated polymerization to form magnetic
Property microballoon.
It is the monodisperse macroporous type polystyrene first prepared to polymerization technique that United States Patent (USP) (US 4,774,265), which discloses,
Microballoon carries out the inside and outside sulfonation in hole or nitrification processing, to make it have hydrophilic interface, adsorbs iron ion, is existed using coprecipitation
Synthesizing magnetic Fe in hole3O4Particulate, then microballoon is swelled, polymerize, wrapped from a kind of monomer containing activity functional groups again
Cover, make microballoon potential close, it is surface-functionalized.
Chinese patent (CN200610027961.7) discloses a kind of use and prepares high magnetic based on miniemulsion-emulsion polymerization
The method of content monodispersity hydrophilicity magnetic composite microsphere, i.e., first by the magnetic ferroferric oxide particle of Coated with Oleic Acid through ultrasound
It is scattered to form nano-scale magnetic droplet, using magnetic droplet as polymerization site, synthesizing magnetic polymer nano-microspheres.But should
Method is confined to synthesize magnetic polymer/SiO 2 composite microsphere of nanoscale, however, limiting extensively should for it
With.
But the distribution of the magnetic microsphere particle diameter of existing preparation is wide, magnetic property is widely different between different microballoons, so as to influence
Its using effect.Therefore, it is materials science field key to be solved to inquire into a kind of preparation method of grain magnetic microsphere
Problem.
The content of the invention
The technical problem to be solved in the present invention is to overcome prior art defect, there is provided a kind of grain magnetic polymer microsphere system
Preparation Method, the uniform particle diameter of the magnetic polymer microsphere prepared using this method, grain diameter is controllable, magnetic is strong.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of grain magnetic polymer microsphere preparation method, comprises the following steps：
(1) at 60-80 DEG C, by Dissolvable Fe3+Salt and enuatrol are reacted in the system of n-hexane and ethanol, and vacuum is done
It is dry, obtain drying iron oleate；
(2) polymer seeds are added in the aqueous solution containing stabilizer, is sufficiently stirred, forms dispersed seed and hang
Supernatant liquid；
(3) iron oleate and monomer are added in stabilizer/solvent mixed solution, stirred, formed iron oleate monomer and hang
Supernatant liquid；
(4) initiator is added in the aqueous solution containing stabilizer, emulsification, forms initiator suspension；
(5) at the polymerization temperature, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid makes kind
Son growth, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, heat up for the first time
Polymerisation, continue to react, you can obtain iron oleate polymer composite microsphere.
(6) second of heating, makes iron oleate pyrolysis synthesizing magnetic nano particle, you can it is micro- to obtain magnetic polymer
Ball.
Preferably, the stabilizer is made up of the surfactant of one or more.It is further preferred that the table
Face activating agent is selected from polyvinyl alcohol, polyvinylpyrrolidone, hydroxymethyl cellulose, oleic acid, oleyl alcohol, hydroxypropyl cellulose or 18
One or more in alcohol.
Preferably, solvent is C1-C3 lower alcohol in step (3).It is further preferred that lower alcohol be low-grade monobasic alcohol or
Dihydric alcohol.
Preferably, polymerization temperature is 70-90 DEG C in step (5), and the temperature of heating is 95-110 DEG C, second liter for the first time
The temperature of temperature is 300-350 DEG C.
Preferably, the polymer seeds are polystyrene seed or styrene-divinylbenzene seed, and the monomer selects
From styrene, divinylbenzene, 2,4 dichloro benzene ethene, acrylic acid, methyl methacrylate, methyl acrylate, ethyl acrylate,
One or more in vinylacetate, GMA or derivatives thereof.
Preferably, the initiator is in benzoyl peroxide, lauroyl peroxide or peroxidating t-butyl formate
It is one or more.
Preferably, the polymer seeds weight accounts for the 40-60% of seed suspension liquid weight, and the iron oleate weight accounts for oil
The 20-40% of sour iron monomer suspension weight, the monomer weight accounts for the 30-60% of iron oleate monomer suspension weight, described
Initiator accounts for the 5-10% of initiator suspension weight.
Preferably, the Dissolvable Fe3+The mol ratio of salt and enuatrol is 1:1.5-1:5.
Preferably, the particle size of the magnetic polymer microsphere is 0.1-200 μm.
The beneficial effect that the present invention is reached：
The uniform particle diameter of magnetic polymer microsphere prepared by the inventive method, grain diameter is controllable, magnetic is strong, and chemically
Matter is stable, has potential application value in food safety detection and biological medicament separation.
Embodiment
With reference to specific embodiment, the invention will be further described.Following examples are only used for clearly illustrating
Technical scheme, and can not be limited the scope of the invention with this.
Embodiment 1
(1) prepare and dry iron oleate, take FeCl3With enuatrol add flask in, and into flask add absolute ethyl alcohol and
The mixed solution of n-hexane, after dissolving, 70 DEG C of heating stirring 4h, the iron oleate for filtering wet, then wet iron oleate is placed in 80
DEG C, 24h is dried in vacuum drying chamber under conditions of vacuum is 100Pa, obtains drying iron oleate；
(2) single dispersing styrene seed (0.55 μm of granularity, CV=3%) is added and contains the water-soluble of polyvinylpyrrolidone
In liquid, stirring is fully dispersed, and it is standby to form seed suspension liquid；
(3) iron oleate and styrene are added in the ethanol containing polyvinylpyrrolidone, is dispersed with stirring uniformly, forms oil
Sour iron monomer suspension is standby；
(4) emulsified after benzoyl peroxide is added in the aqueous solution containing polyvinylpyrrolidone, form initiator and hang
Supernatant liquid is standby；
(5) at 70 DEG C, iron oleate monomer suspension and initiator suspension are added into seed suspension liquid in 180 minutes
In make seed growth, wherein, it be 6.8g/min that iron oleate monomer suspension, which adds speed, and initiator suspension addition speed is
1.01g/min, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, be warming up to
110 DEG C, continue to react 30min, that is, obtain iron oleate polymer composite microsphere；
(6) 320 DEG C are warming up to for the second time, and keeps 2-3h in the case where being kept for 320 DEG C, iron oleate pyrolysis is synthesized magnetic
Property nano particle, you can obtain magnetic polymer microsphere.Magnetic nanoparticle is ferroso-ferric oxide herein.
Its particle diameter is determined using Beckman Counter and particle diameter distribution obtains：Particle diameter is 1.5 μm, CV (coefficient
Of variation) it is 2.9%, magnetic ferroferric oxide accounts for the 40% of whole microspheres weight.
Embodiment 2
(1) prepare and dry iron oleate, take FeCl3With enuatrol add flask in, and into flask add absolute ethyl alcohol and
The mixed solution of n-hexane, after dissolving, 70 DEG C of heating stirring 4h, the iron oleate for filtering wet, then wet iron oleate is placed in 80
DEG C, 24h is dried in vacuum drying chamber under conditions of vacuum is 100Pa, obtains drying iron oleate；
(2) single dispersing styrene-divinylbenzene seed (0.3 μm of granularity, CV=3%) is added and contains hydroxylmethyl cellulose
In the aqueous solution of element, stirring is fully dispersed, and it is standby to form seed suspension liquid；
(3) iron oleate and styrene are added in the ethanol containing hydroxymethyl cellulose, is dispersed with stirring uniformly, forms oleic acid
Iron monomer suspension is standby；
(4) emulsified after benzoyl peroxide is added in the aqueous solution containing hydroxymethyl cellulose, form initiator and suspend
Liquid is standby；
(5) at 80 DEG C, iron oleate monomer suspension and initiator suspension are added into seed suspension liquid in 200 minutes
In make seed growth, wherein, it be 6.5g/min that iron oleate monomer suspension, which adds speed, and initiator suspension addition speed is
0.95g/min, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, be warming up to
100 DEG C, continue to react 40min, that is, obtain iron oleate polymer composite microsphere；
(6) 330 DEG C are warming up to for the second time, and keeps 3h in the case where being kept for 330 DEG C, make iron oleate pyrolysis synthesizing magnetic
Nano particle, you can obtain magnetic polymer microsphere.Magnetic nanoparticle is ferroso-ferric oxide herein.
Its particle diameter is determined using Beckman Counter and particle diameter distribution obtains：Particle size 800nm, CV
(coefficient of variation) is 2.8%, and magnetic ferroferric oxide accounts for the 55% of whole microspheres weight.
Embodiment 3
(1) prepare and dry iron oleate, take FeCl3With enuatrol add flask in, and into flask add absolute ethyl alcohol and
The mixed solution of n-hexane, after dissolving, 70 DEG C of heating stirring 4h, the iron oleate for filtering wet, then wet iron oleate is placed in 70
DEG C, 24h is dried in vacuum drying chamber under conditions of vacuum is 100Pa, obtains drying iron oleate；
(2) single dispersing styrene seed (55 μm of granularity, CV=3%) is added in the aqueous solution containing oleyl alcohol, stirring is filled
It is scattered, it is standby to form seed suspension liquid；
(3) iron oleate and styrene are added in the ethanol containing oleyl alcohol, are dispersed with stirring uniformly, formed iron oleate monomer and hang
Supernatant liquid is standby；
(4) emulsified after benzoyl peroxide is added in the aqueous solution containing oleyl alcohol, it is standby to form initiator suspension；
(5) at 90 DEG C, iron oleate monomer suspension and initiator suspension are added into seed suspension liquid in 200 minutes
In make seed growth, wherein, it be 6.5g/min that iron oleate monomer suspension, which adds speed, and initiator suspension addition speed is
0.95g/min, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, be warming up to
110 DEG C, continue to react 40min, that is, obtain iron oleate polymer composite microsphere；
(6) 350 DEG C are warming up to for the second time, and keeps 2-3h in the case where being kept for 350 DEG C, iron oleate pyrolysis is synthesized magnetic
Property nano particle, you can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Its particle diameter is determined using Beckman Counter and particle diameter distribution obtains：Particle diameter is 110 μm, CV 2.9%, magnetic
Ferroso-ferric oxide accounts for the 56% of whole microspheres weight.
Embodiment 4
(1) prepare and dry iron oleate, take FeCl3With enuatrol add flask in, and into flask add absolute ethyl alcohol and
The mixed solution of n-hexane, after dissolving, 70 DEG C of heating stirring 4h, the iron oleate for filtering wet, then wet iron oleate is placed in 80
DEG C, 24h is dried in vacuum drying chamber under conditions of vacuum is 100Pa, obtains drying iron oleate；
(2) single dispersing styrene seed (15 μm of granularity, CV=3%) is added into the aqueous solution containing polyvinylpyrrolidone
In, stirring is fully dispersed, and it is standby to form seed suspension liquid；
(3) iron oleate and styrene are added in the ethanol containing polyvinylpyrrolidone, is dispersed with stirring uniformly, forms oil
Sour iron monomer suspension is standby；
(4) emulsified after peroxidating t-butyl formate is added in the aqueous solution containing polyvinylpyrrolidone, formed and triggered
Agent suspension is standby；
(5) at 70 DEG C, iron oleate monomer suspension and initiator suspension are added into seed suspension liquid in 180 minutes
In make seed growth, wherein, it be 6.8g/min that iron oleate monomer suspension, which adds speed, and initiator suspension addition speed is
1.01g/min, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, be warming up to
110 DEG C, continue to react 30min, that is, obtain iron oleate polymer composite microsphere；
(6) 320 DEG C are warming up to for the second time, and keeps 2-3h in the case where being kept for 320 DEG C, iron oleate pyrolysis is synthesized magnetic
Property nano particle, you can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Its particle diameter is determined using Beckman Counter and particle diameter distribution obtains：Particle diameter is 33 μm, CV 2.5%, magnetic four
Fe 3 O accounts for the 58% of whole microspheres weight.
Embodiment 5
(1) prepare and dry iron oleate, take FeCl3With enuatrol add flask in, and into flask add absolute ethyl alcohol and
The mixed solution of n-hexane, after dissolving, 70 DEG C of heating stirring 4h, the iron oleate for filtering wet, then wet iron oleate is placed in 80
DEG C, 24h is dried in vacuum drying chamber under conditions of vacuum is 100Pa, obtains drying iron oleate；
(2) single dispersing styrene seed (60 μm of granularity, CV=2.8%) is added and contains the water-soluble of polyvinylpyrrolidone
In liquid, stirring is fully dispersed, and it is standby to form seed suspension liquid；
(3) iron oleate and styrene are added in the ethanol containing polyvinylpyrrolidone, is dispersed with stirring uniformly, forms oil
Sour iron monomer suspension is standby；
(4) emulsified after benzoyl peroxide is added in the aqueous solution containing polyvinylpyrrolidone, form initiator and hang
Supernatant liquid is standby；
(5) at 70 DEG C, iron oleate monomer suspension and initiator suspension are added into seed suspension liquid in 180 minutes
In make seed growth, wherein, it be 6.8g/min that iron oleate monomer suspension, which adds speed, and initiator suspension addition speed is
1.01g/min, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, be warming up to
110 DEG C, continue to react 30min, that is, obtain iron oleate polymer composite microsphere；
(6) 320 DEG C are warming up to for the second time, and keeps 2-3h in the case where being kept for 320 DEG C, iron oleate pyrolysis is synthesized magnetic
Property nano particle, you can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Its particle diameter is determined using Beckman Counter and particle diameter distribution obtains：Particle diameter is 150 μm, CV 2.8%, magnetic
Ferroso-ferric oxide accounts for the 50% of whole microspheres weight.
Embodiment 6
(1) prepare and dry iron oleate, take FeCl3With enuatrol add flask in, and into flask add absolute ethyl alcohol and
The mixed solution of n-hexane, after dissolving, 70 DEG C of heating stirring 4h, the iron oleate for filtering wet, then wet iron oleate is placed in 80
DEG C, 24h is dried in vacuum drying chamber under conditions of vacuum is 100Pa, obtains drying iron oleate；
(2) single dispersing styrene seed (1.5 μm of granularity, CV=3%) is added and contains the water-soluble of polyvinylpyrrolidone
In liquid, stirring is fully dispersed, and it is standby to form seed suspension liquid；
(3) iron oleate and styrene are added in the ethanol containing polyvinylpyrrolidone, is dispersed with stirring uniformly, forms oil
Sour iron monomer suspension is standby；
(4) emulsified after benzoyl peroxide is added in the aqueous solution containing polyvinylpyrrolidone, form initiator and hang
Supernatant liquid is standby；
(5) at 70 DEG C, iron oleate monomer suspension and initiator suspension are added into seed suspension liquid in 180 minutes
In make seed growth, wherein, it be 6.8g/min that iron oleate monomer suspension, which adds speed, and initiator suspension addition speed is
1.01g/min, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, be warming up to
110 DEG C, continue to react 30min, that is, obtain iron oleate polymer composite microsphere；
(6) 320 DEG C are warming up to for the second time, and keeps 2-3h in the case where being kept for 320 DEG C, iron oleate pyrolysis is synthesized magnetic
Property nano particle, you can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Its particle diameter is determined using Beckman Counter and particle diameter distribution obtains：Particle diameter is 4.5 μm, CV 2.6%, magnetic
Ferroso-ferric oxide accounts for the 55% of whole microspheres weight.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvement and deformation can also be made, these are improved and deformation
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of grain magnetic polymer microsphere preparation method, it is characterised in that comprise the following steps：
(1) at 60-80 DEG C, by Dissolvable Fe3+Salt and enuatrol react in the system of n-hexane and ethanol, vacuum drying,
Obtain drying iron oleate；
(2) polymer seeds are added in the aqueous solution containing stabilizer, is sufficiently stirred, forms dispersed seed suspension
Liquid；
(3) iron oleate and monomer are added in stabilizer/solvent mixed solution, stirred, form iron oleate monomer suspension；
(4) initiator is added in the aqueous solution containing stabilizer, emulsification, forms initiator suspension；
(5) at the polymerization temperature, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid gives birth to seed
It is long, stop adding iron oleate monomer suspension and initiator suspension after reaching default microspherulite diameter, heating polymerization for the first time
Reaction, continues to react, you can obtain iron oleate polymer composite microsphere；
(6) second of heating, makes iron oleate pyrolysis synthesizing magnetic nano particle, you can obtain magnetic polymer microsphere.
A kind of 2. grain magnetic polymer microsphere preparation method according to claim 1, it is characterised in that the stabilizer
It is made up of the surfactant of one or more.
3. a kind of grain magnetic polymer microsphere preparation method according to claim 2, it is characterised in that in step (3)
Solvent is C1-C3 lower alcohol.
4. a kind of grain magnetic polymer microsphere preparation method according to claim 3, it is characterised in that in step (5)
Polymerization temperature is 70-90 DEG C, and the temperature of heating is 95-110 DEG C for the first time, and the temperature of second of heating is 300-350 DEG C.
5. a kind of grain magnetic polymer microsphere preparation method according to claim 2, it is characterised in that live on the surface
Property agent is in polyvinyl alcohol, polyvinylpyrrolidone, hydroxymethyl cellulose, oleic acid, oleyl alcohol, hydroxypropyl cellulose or octadecyl alcolol
One or more.
A kind of 6. grain magnetic polymer microsphere preparation method according to claim any one of 1-5, it is characterised in that institute
It is polystyrene seed or styrene-divinylbenzene seed to state polymer seeds, and the monomer is selected from styrene, divinyl
Benzene, 2,4 dichloro benzene ethene, acrylic acid, methyl methacrylate, methyl acrylate, ethyl acrylate, vinylacetate, methyl
One or more in glycidyl acrylate.
A kind of 7. grain magnetic polymer microsphere preparation method according to claim 6, it is characterised in that the initiator
One or more in benzoyl peroxide, lauroyl peroxide or peroxidating t-butyl formate.
A kind of 8. grain magnetic polymer microsphere preparation method according to claim any one of 1-5, it is characterised in that institute
The 40-60% that polymer seeds weight accounts for seed suspension liquid weight is stated, the iron oleate weight accounts for iron oleate monomer suspension weight
The 20-40% of amount, the monomer weight account for the 30-60% of iron oleate monomer suspension weight, and the initiator accounts for initiator and hanged
The 5-10% of supernatant liquid weight.
A kind of 9. grain magnetic polymer microsphere preparation method according to claim 1, it is characterised in that the solubility
Fe3+The mol ratio of salt and enuatrol is 1:1.5-1:5.
A kind of 10. grain magnetic polymer microsphere preparation method according to claim 1, it is characterised in that the magnetic
The particle size of polymer microballoon is 0.1-200 μm.
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