CN105754021A - Method for preparing mean-particle magnetic polymer microsphere - Google Patents
Method for preparing mean-particle magnetic polymer microsphere Download PDFInfo
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- CN105754021A CN105754021A CN201610329610.5A CN201610329610A CN105754021A CN 105754021 A CN105754021 A CN 105754021A CN 201610329610 A CN201610329610 A CN 201610329610A CN 105754021 A CN105754021 A CN 105754021A
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- 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
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- 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
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- 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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- 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
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- 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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Abstract
The invention discloses a method for preparing mean-particle magnetic polymer microspheres. The method comprises the following steps: preparing ferric oleate, preparing polymer seed suspension, preparing ferric oleate and monomer suspension, preparing initiator suspension, adding the ferric oleate and monomer suspension and the initiator suspension into the seed suspension at a polymerization temperature so as to enable seeds to grow, after reaching a preset microsphere particle size, stopping adding the ferric oleate and monomer suspension and the initiator suspension, performing first temperature rise polymerization reaction, and enabling the components to react continuously, thereby obtaining ferric oleate polymer composite microspheres. The magnetic polymer microspheres prepared by using the method are uniform in particle size, controllable in particle size and strong in magnetism.
Description
Technical field
The present invention relates to a kind of all grain magnetic polymer microsphere preparation methoies, belong to technical field of polymer materials.
Background technology
Magnetic microsphere has a wide range of applications in bio-separation engineering and biomedical engineering, has tempting application prospect separating in the fields such as purification of nucleic acid extraction, cell separation, immobilized enzyme, immune detection, targeted drug, protein and enzyme especially.
The method of prior art synthesizing magnetic polymer microballoon mainly has investment, monomer polymerization method and interfacial deposition method etc..
United States Patent (USP) (US4,339,337 and US4,358,388) disclosing suspension polymerization and micro-suspension polymerization, the oil phase of magnetic four ferric oxide particles, lipophile vinyl monomer and the oil-soluble initiator composition that namely oleophylicization are processed is dispersed in aqueous phase, under the effect of mechanical agitation and stabilizer, oil phase is that drop state is dispersed in aqueous phase, adds thermal-initiated polymerization and forms magnetic microsphere.
United States Patent (USP) (US4,774,265) disclose the monodisperse macroporous type polystyrene microsphere being first prepared by polymerization technique and carry out the inside and outside sulfonation in hole or nitration treatment, to make it have hydrophilic interface, absorption iron ion, adopts coprecipitation synthesizing magnetic Fe in hole3O4Microgranule, then select again a kind of monomer containing activity functional groups microsphere is carried out swelling, polymerization, cladding, make microsphere potential close, surface-functionalized.
Chinese patent (CN200610027961.7) discloses a kind of method that employing prepares high magnetic content monodispersity hydrophilicity magnetic composite microsphere based on miniemulsion-emulsion polymerization, namely first the magnetic ferroferric oxide granule of Coated with Oleic Acid is formed nano-scale magnetic droplet through ultrasonic disperse, with magnetic droplet for polymerization site, synthesizing magnetic polymer nano-microspheres.But the method is confined to the magnetic polymer/SiO 2 composite microsphere of synthesis nanoscale, but, limit its extensive use.
But the magnetic microsphere particle diameter of existing preparation distribution width, between different microspheres, magnetic property is widely different, thus have impact on its result of use.Therefore, inquiring into the preparation method of a kind of equal grain magnetic microsphere is material science key issue to be solved.
Summary of the invention
The technical problem to be solved in the present invention is to overcome prior art defect, it is provided that a kind of all grain magnetic polymer microsphere preparation methoies, uses the uniform particle diameter of magnetic polymer microsphere prepared by the method, grain diameter is controlled, magnetic is strong.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of all grain magnetic polymer microsphere preparation methoies, comprise the following steps:
(1) at 60-80 DEG C, by Dissolvable Fe3+Salt and enuatrol react in the system of normal hexane and ethanol, vacuum drying, obtain dry iron oleate；
(2) polymer seeds is added in the aqueous solution containing stabilizer, be sufficiently stirred for, form homodisperse seed suspension liquid；
(3) iron oleate and monomer are added in stabilizer/solvent mixed solution, stir, form iron oleate monomer suspension；
(4) initiator is added in the aqueous solution containing stabilizer, emulsifying, form initiator suspension；
(5) at the polymerization temperature, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and makes seed growth, stop adding iron oleate monomer suspension and initiator suspension after reaching the microspherulite diameter preset, heat up polyreaction for the first time, continue reaction, iron oleate polymer composite microsphere can be obtained.
(6) second time heats up, and makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.
Preferably, described stabilizer is made up of one or more surfactant.It is further preferred that described surfactant is selected from one or more in polyvinyl alcohol, polyvinylpyrrolidone, hydroxymethyl cellulose, oleic acid, oleyl alcohol, hydroxypropyl cellulose or octadecanol.
Preferably, in step (3), solvent is the lower alcohol of C1-C3.It is further preferred that lower alcohol is low-grade monobasic alcohol or dihydroxylic alcohols.
Preferably, in step (5), polymerization temperature is 70-90 DEG C, and the temperature that first time heats up is 95-110 DEG C, and the temperature that second time heats up is 300-350 DEG C.
Preferably, described polymer seeds is polystyrene seed or styrene-divinylbenzene seed, described monomer is selected from one or more in styrene, divinylbenzene, 2,4-dichlorostyrenes, acrylic acid, methyl methacrylate, acrylic acid methyl ester., ethyl acrylate, vinylacetate, glycidyl methacrylate or derivatives thereof.
Preferably, described initiator is selected from one or more in benzoyl peroxide, lauroyl peroxide or peroxidating t-butyl formate.
Preferably, described polymer seeds weight accounts for the 40-60% of seed suspension liquid weight, described iron oleate weight accounts for the 20-40% of iron oleate monomer suspension weight, and described monomer weight accounts for the 30-60% of iron oleate monomer suspension weight, and described initiator accounts for the 5-10% of initiator suspension weight.
Preferably, described Dissolvable Fe3+The mol ratio of salt and enuatrol is 1:1.5-1:5.
Preferably, the size of described magnetic polymer microsphere is 0.1-200 μm.
The beneficial effect that the present invention reaches:
The uniform particle diameter of magnetic polymer microsphere prepared by the inventive method, grain diameter are controlled, magnetic is strong, and stable chemical nature, have potential using value with biological medicament in food safety detection separates.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.Following example are only for clearly illustrating technical scheme, and can not limit the scope of the invention with this.
Embodiment 1
(1) the dry iron oleate of preparation, takes FeCl3Add in flask with enuatrol, and in flask, add the mixed solution of dehydrated alcohol and normal hexane, after dissolving, 70 DEG C of heated and stirred 4h, the iron oleate filtering wet, wetter iron oleate is placed in 80 DEG C, vacuum drying oven inner drying 24h when vacuum is 100Pa, obtains dry iron oleate；
(2) single dispersing styrene seed (granularity 0.55 μm, CV=3%) is added in the aqueous solution containing polyvinylpyrrolidone, stir fully dispersed, form seed suspension liquid standby；
(3) adding in the ethanol containing polyvinylpyrrolidone by iron oleate and styrene, dispersed with stirring is uniform, forms iron oleate monomer suspension standby；
(4) benzoyl peroxide is added emulsifying after in the aqueous solution containing polyvinylpyrrolidone, form initiator suspension standby；
(5) at 70 DEG C, in 180 minutes, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and make seed growth, wherein, it is 6.8g/min that iron oleate monomer suspension adds speed, it is 1.01g/min that initiator suspension adds speed, stops adding iron oleate monomer suspension and initiator suspension, be warming up to 110 DEG C after reaching the microspherulite diameter preset, continue reaction 30min, namely obtain iron oleate polymer composite microsphere；
(6) second time is warming up to 320 DEG C, and keeps 2-3h at keeping 320 DEG C, makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.Magnetic nanoparticle is ferroso-ferric oxide herein.
Adopt BeckmanCounter to measure its particle diameter and particle size distribution obtains: particle diameter is 1.5 μm, and CV (coefficientofvariation) is 2.9%, and magnetic ferroferric oxide accounts for the 40% of whole microspheres weight.
Embodiment 2
(1) the dry iron oleate of preparation, takes FeCl3Add in flask with enuatrol, and in flask, add the mixed solution of dehydrated alcohol and normal hexane, after dissolving, 70 DEG C of heated and stirred 4h, the iron oleate filtering wet, wetter iron oleate is placed in 80 DEG C, vacuum drying oven inner drying 24h when vacuum is 100Pa, obtains dry iron oleate；
(2) single dispersing styrene-divinylbenzene seed (granularity 0.3 μm, CV=3%) is added in the aqueous solution containing hydroxymethyl cellulose, stir fully dispersed, form seed suspension liquid standby；
(3) adding in the ethanol containing hydroxymethyl cellulose by iron oleate and styrene, dispersed with stirring is uniform, forms iron oleate monomer suspension standby；
(4) benzoyl peroxide is added emulsifying after in the aqueous solution containing hydroxymethyl cellulose, form initiator suspension standby；
(5) at 80 DEG C, in 200 minutes, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and make seed growth, wherein, it is 6.5g/min that iron oleate monomer suspension adds speed, it is 0.95g/min that initiator suspension adds speed, stops adding iron oleate monomer suspension and initiator suspension, be warming up to 100 DEG C after reaching the microspherulite diameter preset, continue reaction 40min, namely obtain iron oleate polymer composite microsphere；
(6) second time is warming up to 330 DEG C, and keeps 3h at keeping 330 DEG C, makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.Magnetic nanoparticle is ferroso-ferric oxide herein.
Adopt BeckmanCounter to measure its particle diameter and particle size distribution obtains: size 800nm, CV (coefficientofvariation) are 2.8%, and magnetic ferroferric oxide accounts for the 55% of whole microspheres weight.
Embodiment 3
(1) the dry iron oleate of preparation, takes FeCl3Add in flask with enuatrol, and in flask, add the mixed solution of dehydrated alcohol and normal hexane, after dissolving, 70 DEG C of heated and stirred 4h, the iron oleate filtering wet, wetter iron oleate is placed in 70 DEG C, vacuum drying oven inner drying 24h when vacuum is 100Pa, obtains dry iron oleate；
(2) single dispersing styrene seed (granularity 55 μm, CV=3%) is added in the aqueous solution containing oleyl alcohol, stir fully dispersed, form seed suspension liquid standby；
(3) adding in the ethanol containing oleyl alcohol by iron oleate and styrene, dispersed with stirring is uniform, forms iron oleate monomer suspension standby；
(4) benzoyl peroxide is added emulsifying after in the aqueous solution containing oleyl alcohol, form initiator suspension standby；
(5) at 90 DEG C, in 200 minutes, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and make seed growth, wherein, it is 6.5g/min that iron oleate monomer suspension adds speed, it is 0.95g/min that initiator suspension adds speed, stops adding iron oleate monomer suspension and initiator suspension, be warming up to 110 DEG C after reaching the microspherulite diameter preset, continue reaction 40min, namely obtain iron oleate polymer composite microsphere；
(6) second time is warming up to 350 DEG C, and keeps 2-3h at keeping 350 DEG C, makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Adopt BeckmanCounter to measure its particle diameter and particle size distribution obtains: particle diameter is 110 μm, and CV is 2.9%, and magnetic ferroferric oxide accounts for the 56% of whole microspheres weight.
Embodiment 4
(1) the dry iron oleate of preparation, takes FeCl3Add in flask with enuatrol, and in flask, add the mixed solution of dehydrated alcohol and normal hexane, after dissolving, 70 DEG C of heated and stirred 4h, the iron oleate filtering wet, wetter iron oleate is placed in 80 DEG C, vacuum drying oven inner drying 24h when vacuum is 100Pa, obtains dry iron oleate；
(2) single dispersing styrene seed (granularity 15 μm, CV=3%) is added in the aqueous solution containing polyvinylpyrrolidone, stir fully dispersed, form seed suspension liquid standby；
(3) adding in the ethanol containing polyvinylpyrrolidone by iron oleate and styrene, dispersed with stirring is uniform, forms iron oleate monomer suspension standby；
(4) peroxidating t-butyl formate is added emulsifying after in the aqueous solution containing polyvinylpyrrolidone, form initiator suspension standby；
(5) at 70 DEG C, in 180 minutes, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and make seed growth, wherein, it is 6.8g/min that iron oleate monomer suspension adds speed, it is 1.01g/min that initiator suspension adds speed, stops adding iron oleate monomer suspension and initiator suspension, be warming up to 110 DEG C after reaching the microspherulite diameter preset, continue reaction 30min, namely obtain iron oleate polymer composite microsphere；
(6) second time is warming up to 320 DEG C, and keeps 2-3h at keeping 320 DEG C, makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Adopt BeckmanCounter to measure its particle diameter and particle size distribution obtains: particle diameter is 33 μm, and CV is 2.5%, and magnetic ferroferric oxide accounts for the 58% of whole microspheres weight.
Embodiment 5
(1) the dry iron oleate of preparation, takes FeCl3Add in flask with enuatrol, and in flask, add the mixed solution of dehydrated alcohol and normal hexane, after dissolving, 70 DEG C of heated and stirred 4h, the iron oleate filtering wet, wetter iron oleate is placed in 80 DEG C, vacuum drying oven inner drying 24h when vacuum is 100Pa, obtains dry iron oleate；
(2) single dispersing styrene seed (granularity 60 μm, CV=2.8%) is added in the aqueous solution containing polyvinylpyrrolidone, stir fully dispersed, form seed suspension liquid standby；
(3) adding in the ethanol containing polyvinylpyrrolidone by iron oleate and styrene, dispersed with stirring is uniform, forms iron oleate monomer suspension standby；
(4) benzoyl peroxide is added emulsifying after in the aqueous solution containing polyvinylpyrrolidone, form initiator suspension standby；
(5) at 70 DEG C, in 180 minutes, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and make seed growth, wherein, it is 6.8g/min that iron oleate monomer suspension adds speed, it is 1.01g/min that initiator suspension adds speed, stops adding iron oleate monomer suspension and initiator suspension, be warming up to 110 DEG C after reaching the microspherulite diameter preset, continue reaction 30min, namely obtain iron oleate polymer composite microsphere；
(6) second time is warming up to 320 DEG C, and keeps 2-3h at keeping 320 DEG C, makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Adopt BeckmanCounter to measure its particle diameter and particle size distribution obtains: particle diameter is 150 μm, and CV is 2.8%, and magnetic ferroferric oxide accounts for the 50% of whole microspheres weight.
Embodiment 6
(1) the dry iron oleate of preparation, takes FeCl3Add in flask with enuatrol, and in flask, add the mixed solution of dehydrated alcohol and normal hexane, after dissolving, 70 DEG C of heated and stirred 4h, the iron oleate filtering wet, wetter iron oleate is placed in 80 DEG C, vacuum drying oven inner drying 24h when vacuum is 100Pa, obtains dry iron oleate；
(2) single dispersing styrene seed (granularity 1.5 μm, CV=3%) is added in the aqueous solution containing polyvinylpyrrolidone, stir fully dispersed, form seed suspension liquid standby；
(3) adding in the ethanol containing polyvinylpyrrolidone by iron oleate and styrene, dispersed with stirring is uniform, forms iron oleate monomer suspension standby；
(4) benzoyl peroxide is added emulsifying after in the aqueous solution containing polyvinylpyrrolidone, form initiator suspension standby；
(5) at 70 DEG C, in 180 minutes, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and make seed growth, wherein, it is 6.8g/min that iron oleate monomer suspension adds speed, it is 1.01g/min that initiator suspension adds speed, stops adding iron oleate monomer suspension and initiator suspension, be warming up to 110 DEG C after reaching the microspherulite diameter preset, continue reaction 30min, namely obtain iron oleate polymer composite microsphere；
(6) second time is warming up to 320 DEG C, and keeps 2-3h at keeping 320 DEG C, makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.Secondary magnetic nanoparticle of eating is ferroso-ferric oxide.
Adopt BeckmanCounter to measure its particle diameter and particle size distribution obtains: particle diameter is 4.5 μm, and CV is 2.6%, and magnetic ferroferric oxide accounts for the 55% of whole microspheres weight.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the technology of the present invention principle; can also making some improvement and deformation, these improve and deformation also should be regarded as protection scope of the present invention.
Claims (10)
1. an equal 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 normal hexane and ethanol, vacuum drying, obtain dry iron oleate；
(2) polymer seeds is added in the aqueous solution containing stabilizer, be sufficiently stirred for, form homodisperse seed suspension liquid；
(3) iron oleate and monomer are added in stabilizer/solvent mixed solution, stir, form iron oleate monomer suspension；
(4) initiator is added in the aqueous solution containing stabilizer, emulsifying, form initiator suspension；
(5) at the polymerization temperature, iron oleate monomer suspension and initiator suspension are added in seed suspension liquid and makes seed growth, stop adding iron oleate monomer suspension and initiator suspension after reaching the microspherulite diameter preset, heat up polyreaction for the first time, continue reaction, iron oleate polymer composite microsphere can be obtained；
(6) second time heats up, and makes iron oleate pyrolysis synthesizing magnetic nano-particle, can obtain magnetic polymer microsphere.
2. the equal grain magnetic polymer microsphere preparation method of one according to claim 1, it is characterised in that described stabilizer is made up of one or more surfactant.
3. the equal grain magnetic polymer microsphere preparation method of one according to claim 2, it is characterised in that in step (3), solvent is the lower alcohol of C1-C3.
4. the equal grain magnetic polymer microsphere preparation method of one according to claim 3, it is characterised in that in step (5), polymerization temperature is 70-90 DEG C, the temperature that first time heats up is 95-110 DEG C, and the temperature that second time heats up is 300-350 DEG C.
5. the equal grain magnetic polymer microsphere preparation method of one according to claim 2, it is characterized in that, described surfactant is selected from one or more in polyvinyl alcohol, polyvinylpyrrolidone, hydroxymethyl cellulose, oleic acid, oleyl alcohol, hydroxypropyl cellulose or octadecanol.
6. a kind of all grain magnetic polymer microsphere preparation methoies according to any one of claim 1-5, it is characterized in that, described polymer seeds is polystyrene seed or styrene-divinylbenzene seed, described monomer is selected from one or more in styrene, divinylbenzene, 2,4-dichlorostyrenes, acrylic acid, methyl methacrylate, acrylic acid methyl ester., ethyl acrylate, vinylacetate, glycidyl methacrylate or derivatives thereof.
7. the equal grain magnetic polymer microsphere preparation method of one according to claim 6, it is characterised in that described initiator is selected from one or more in benzoyl peroxide, lauroyl peroxide or peroxidating t-butyl formate.
8. a kind of all grain magnetic polymer microsphere preparation methoies according to any one of claim 1-5, it is characterized in that, described polymer seeds weight accounts for the 40-60% of seed suspension liquid weight, described iron oleate weight accounts for the 20-40% of iron oleate monomer suspension weight, described monomer weight accounts for the 30-60% of iron oleate monomer suspension weight, and described initiator accounts for the 5-10% of initiator suspension weight.
9. the equal grain magnetic polymer microsphere preparation method of one according to claim 1, it is characterised in that described Dissolvable Fe3+The mol ratio of salt and enuatrol is 1:1.5-1:5.
10. the equal grain magnetic polymer microsphere preparation method of one according to claim 1, it is characterised in that the size of described magnetic polymer microsphere is 0.1-200 μm.
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| CN110294816A (en) * | 2019-06-06 | 2019-10-01 | 东莞东阳光科研发有限公司 | Magnetic Nano polystyrene carboxyl microballoon and preparation method thereof |
| CN110511309A (en) * | 2019-09-06 | 2019-11-29 | 无锡迈科为生物科技有限公司 | A kind of preparation method of magnetic macromolecular microsphere |
| CN111892033A (en) * | 2020-07-24 | 2020-11-06 | 无锡迈科为生物科技有限公司 | Preparation method of hydroxyapatite microspheres |
| CN112023841A (en) * | 2020-07-24 | 2020-12-04 | 无锡迈科为生物科技有限公司 | Preparation method of uniform magnetic microspheres for extracting high-load nucleic acid |
| CN114073940A (en) * | 2020-08-20 | 2022-02-22 | 清华大学 | Core-shell particles and preparation method thereof |
| CN114247393A (en) * | 2021-12-22 | 2022-03-29 | 苏州知益微球科技有限公司 | Magnetic polymer microsphere and preparation method and application thereof |
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