CN101071669A - Method for preparing magnetic compound micro-sphere with core-shell structure by electron beam irradiation - Google Patents
Method for preparing magnetic compound micro-sphere with core-shell structure by electron beam irradiation Download PDFInfo
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- CN101071669A CN101071669A CN 200710038786 CN200710038786A CN101071669A CN 101071669 A CN101071669 A CN 101071669A CN 200710038786 CN200710038786 CN 200710038786 CN 200710038786 A CN200710038786 A CN 200710038786A CN 101071669 A CN101071669 A CN 101071669A
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Abstract
This invention involves a core-shell structure of the magnetic composite microspheres method by electron beam irradiation, primarily caused by electron beam monomer polymerization approach to the preparation of magnetic composites, which belongs to magnetic composites manufacturing process technology. This invention's steps are as following: first using coprecipitation with ferrous sulfate and ferric chloride as raw material obtained magnetic Fe3O4 nanoparticles, the size of 5 to 12 nm, and the preparation of its pH = 4 acidic magnetic fluid; then acrylamide monomer and crosslinking agent N, N-methyl-double the proportion of acrylamide in accordance with the regulations by adding dispersed into the water; Fe3O4, acrylamide monomer, N, N-methyl acrylamide three pairs in the mixed solution of the concentration ratio of the weight of 11:1000: 1; the mixture placed in polyethylene bags , and then placed in electron beam irradiation under irradiation, the total radiation dose is 20 KGy; finally core-shell structure of the magnetic composite microspheres can be gaint and microsphere diameter 0.2 to 1.0 mu m.
Description
Technical field
The present invention relates to a kind of method that adopts prepared by EB irradiation to have the magnetic composite microsphere of nucleocapsid structure, mainly is to adopt the method for electron beam trigger monomer polymerization to prepare magnetic composite, belongs to the magnetic composite manufacturing process technology field.
Background technology
Magnetic composite microsphere is a kind of new function material that latest developments are got up, and being does not have formed material by suitable method with macromolecular material and magnetic to combine and form the magnetic composite microsphere with a fixed structure and characteristic.Because of magnetic composite microsphere has the numerous features and the magnetic correspondence of common polymer microsphere concurrently, not only can give its surface functional group by methods such as copolymerization and surface modifications thereof, can also under external magnetic field, separate easily; Thereby have wide practical use in fields such as biogenetic products separation and purification, immobilised enzymes, organic synthesis catalysis, target medicine carriers.
The preparation method of magnetic composite microsphere mainly contains: investment, monomer polymerization method, in-situ chemical conversion method, biological synthesis process etc.Monomer polymerization method is maximum method for preparing magnetic composite microsphere of using at present, but all is at present with the polymerization of initator trigger monomer, will inevitably cause initator residual, and this has just limited the range of application of product; And its required reaction time is longer.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts prepared by EB irradiation to have the magnetic composite microsphere of nucleocapsid structure, mainly is the method that adopts the polymerization of electron beam spoke trigger monomer, it is characterized in that having following technical process and step:
A. be raw material with iron chloride and ferrous sulfate at first, under nitrogen atmosphere, add concentrated ammonia liquor, stir and be warming up to 80 ℃, make it reaction with coprecipitation; Reaction finishes the back and isolates black solid product Fe with permanent magnet
3O
4Nano particle, its particle diameter are 5～12nm; With this nanometer Fe
3O
4Be dissolved in tri-distilled water, use salt acid for adjusting pH value to 4 again, stand-by;
B. with above-mentioned Fe
3O
4Magnetic nano-particle is a kernel, is the magnetic composite microsphere that shell is made nucleocapsid structure with the polyacrylamide: adopt a certain amount of acrylamide monomer, nanometer Fe
3O
4With crosslinking agent N, the N-methylene-bisacrylamide is a reactive material, and three's weight concentration ratio is 1000: 1: 11; The pH value of conditioned reaction solution extremely
6; Mixed solution is positioned in the Polythene Bag, and charges into high pure nitrogen in bag, sealing is placed on electronics and adds
Carry out irradiation under the electron beam that the speed device produces, electronic beam current intensity is 0.5mA, and total radiation dosage is 20KGy;
C. the product behind irradiation placed 1mol/L salt acid soak 24 hours, removed the Fe that does not coat
3O
4Under the action of a magnetic field,, isolate the acrylamide monomer and the homopolymers thereof that have neither part nor lot in coating reaction with tri-distilled water and absolute ethyl alcohol cyclic washing;
D. above-mentioned product is carried out vacuumize at 40 ℃, through grinding, finally obtain the magnetic composite microsphere of nucleocapsid structure again.
The inventive method adopts radiation polymerization, utilizes on monomer, to produce the free radical activity point on the accelerator electron beam, thereby at the magnetic particle surface aggregate.
The characteristics and the advantage of the inventive method are as follows:
(1) the inventive method adopts electron beam substituted chemistry initator to realize monomer polymerization, can not cause initator residual, can make pure magnetic composite microsphere; In addition, because the energy of electron beam is very high, reaction can be finished rapidly at normal temperatures.
(2) the magnetic core-shell particles that makes, its shell coating layer is tight, the chemical stability height, oxidation resistance is strong.
(3) the magnetic core-shell particles that makes, its magnetic field intensity is bigger, and very strong magnetic responsiveness ability is arranged.
(4) the magnetic core-shell particles good dispersion in water that makes, and the easily further functionalization of its surperficial polyacrylamide, can connect various bioactivators and drug molecule after the modification, be adapted to separating and purifying of various biomaterials and pharmaceutical products, and can be used as biomolecule and the directed carrier of carrying of drug molecule magnetic control.
Embodiment
After now embodiments of the invention specifically being described in.
Embodiment 1
The technical process and the step of present embodiment are as described below:
(1) takes by weighing the FeCl of 2.144g
36H
2The FeSO of O and 1.112g
47H
2O is soluble in water, make dissolving fully with ultrasonic agitation, be made into 100mol solution, to add concentration expressed in percentage by weight under the pure nitrogen gas state in solution fast be 28% concentrated ammonia liquor stirring and feed then, be reflected at carry out 15 minutes under 55 ℃ of temperature after, be warming up to 80 ℃, under vigorous stirring, keep isothermal reaction 1 hour at 80 ℃; Reaction finishes the back and separates black solid product Fe with permanent magnet
3O
4Nano particle, its particle diameter are 5～12nm, with this nanometer Fe
3O
4Be dissolved in tri-distilled water, use salt acid for adjusting pH value to 4 again, the solution solid content is 10g/L, and is stand-by.
(2) take by weighing the crosslinking agent N of 2.757g monomer acrylamide and 0.003g, the N-methylene-bisacrylamide is measured above-mentioned Fe again
3O
4Nano-particle solution 3ml, with above-mentioned three kinds of material mixed dissolutions in the 200ml deionized water, stirred 10 minutes under the 400rpm rotating speed with mixer, then mixed solution is positioned in the polyethylene bag, and in bag, charges into high pure nitrogen, after 10 minutes, with its sealing, be positioned over subsequently under the electron beam that electron accelerator produces and carry out irradiation, electronic beam current intensity is 0.5mA, and total radiation dosage is 20KGy;
(3) product behind irradiation places 1mol/L hydrochloric acid to soak 24 hours, removes the Fe that does not coat
3O
4, with tri-distilled water washing 3 times, use absolute ethanol washing again 2 times then, have neither part nor lot in the acrylamide monomer and the homopolymers thereof of coating reaction with removal;
(4) isolate Fe with high-intensity magnetic field
3O
4/ polyacrolein amine magnetic core-shell particles; It is carried out vacuumize under 40 ℃,, finally obtain the magnetic composite microsphere of nucleocapsid structure again through pulverizing.Little bulb diameter is between 0.2～1.0 μ m.
Claims (1)
1. method that adopts prepared by EB irradiation to have the magnetic composite microsphere of nucleocapsid structure is characterized in that having following technical process and step:
A. be raw material with iron chloride and ferrous sulfate at first, under nitrogen atmosphere, add concentrated ammonia liquor, stir and be warming up to 80 ℃, make it reaction with coprecipitation; Reaction finishes the back and isolates black solid product Fe with permanent magnet
3O
4Nano particle, its particle diameter are 5～12nm; With this nanometer Fe
3O
4Be dissolved in tri-distilled water, use salt acid for adjusting pH value to 4 again, stand-by;
B. with above-mentioned Fe
3O
4Magnetic nano-particle is a kernel, is the magnetic composite microsphere that shell is made nucleocapsid structure with the polyacrylamide: adopt a certain amount of acrylamide monomer, nanometer Fe
3O
4With crosslinking agent N, the N-methylene-bisacrylamide is a reactive material, and three's weight concentration ratio is 1000: 1: 11; The pH value to 6 of conditioned reaction solution; Mixed solution is positioned in the Polythene Bag, and charges into high pure nitrogen in bag, seal under the electron beam that is placed on the electron accelerator generation and carry out irradiation, electronic beam current intensity is 0.5mA, and total radiation dosage is 20KGy;
C. the product behind irradiation placed 1mol/L salt acid soak 24 hours, removed the Fe that does not coat
3O
4Under the action of a magnetic field,, isolate the acrylamide monomer and the homopolymers thereof that have neither part nor lot in coating reaction with tri-distilled water and absolute ethyl alcohol cyclic washing;
D. above-mentioned product is carried out vacuumize at 40 ℃, through grinding, finally obtain the magnetic composite microsphere of nucleocapsid structure again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710038786 CN101071669A (en) | 2007-03-29 | 2007-03-29 | Method for preparing magnetic compound micro-sphere with core-shell structure by electron beam irradiation |
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|---|---|---|---|
| CN 200710038786 CN101071669A (en) | 2007-03-29 | 2007-03-29 | Method for preparing magnetic compound micro-sphere with core-shell structure by electron beam irradiation |
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| CN101071669A true CN101071669A (en) | 2007-11-14 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130937A (en) * | 2013-02-07 | 2013-06-05 | 东华大学 | Preparing method of ferroferric oxide functionalized nanometer materials coated by polyacrylamide (PAM) |
| CN106220796A (en) * | 2016-08-29 | 2016-12-14 | 河南省计量科学研究院 | A kind of radiation method preparation method of the magnetic microsphere separated for bioprotein |
| CN106848263A (en) * | 2017-03-25 | 2017-06-13 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction liquid phase synthesis C/Ag, Bi/BiF3Compound fluorination bismuth anode material for lithium-ion batteries and preparation method thereof |
| CN106876681A (en) * | 2017-03-25 | 2017-06-20 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction liquid phase synthesis C/Bi/BiF3Compound fluorination bismuth anode material for lithium-ion batteries and preparation method thereof |
| CN106876706A (en) * | 2017-03-25 | 2017-06-20 | 宁波吉电鑫新材料科技有限公司 | A kind of monolithic conductive original position C/Bi/BiF3Compound fluorination bismuth anode material for lithium-ion batteries and preparation method thereof |
| CN106953083A (en) * | 2017-03-25 | 2017-07-14 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction original position C/ metal solid solutions/Ni2+,Ca2+Adulterate BiF3Positive pole and preparation method |
| CN106953085A (en) * | 2017-03-25 | 2017-07-14 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction original position C/Ag, metal solid solution/Mg2+Adulterate BiF3Positive pole and preparation method |
| CN109603775A (en) * | 2018-11-30 | 2019-04-12 | 武汉理工大学 | A kind of carrying metal ion polyacrylamide magnetic bead and its preparation method and application |
| CN110721644A (en) * | 2019-10-22 | 2020-01-24 | 北京理工大学 | Radiation preparation method of vinyl polymer microcapsule |
| CN110833802A (en) * | 2018-08-15 | 2020-02-25 | 漯河医学高等专科学校 | Method for preparing magnetic starch microspheres by gamma-ray irradiation |
| CN113861469A (en) * | 2021-10-19 | 2021-12-31 | 中国工程物理研究院激光聚变研究中心 | Preparation method of superparamagnetic polyimide composite film |
| CN116764634A (en) * | 2022-03-11 | 2023-09-19 | 大庆油田有限责任公司 | Ionizing radiation catalyst, polyacrylamide solution and viscosity reduction method for polymer-containing sewage in oil field |
-
2007
- 2007-03-29 CN CN 200710038786 patent/CN101071669A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130937A (en) * | 2013-02-07 | 2013-06-05 | 东华大学 | Preparing method of ferroferric oxide functionalized nanometer materials coated by polyacrylamide (PAM) |
| CN106220796A (en) * | 2016-08-29 | 2016-12-14 | 河南省计量科学研究院 | A kind of radiation method preparation method of the magnetic microsphere separated for bioprotein |
| CN106220796B (en) * | 2016-08-29 | 2018-07-17 | 河南省计量科学研究院 | A kind of radiation method preparation method of magnetic microsphere for bioprotein separation |
| CN106953085A (en) * | 2017-03-25 | 2017-07-14 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction original position C/Ag, metal solid solution/Mg2+Adulterate BiF3Positive pole and preparation method |
| CN106876706A (en) * | 2017-03-25 | 2017-06-20 | 宁波吉电鑫新材料科技有限公司 | A kind of monolithic conductive original position C/Bi/BiF3Compound fluorination bismuth anode material for lithium-ion batteries and preparation method thereof |
| CN106953083A (en) * | 2017-03-25 | 2017-07-14 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction original position C/ metal solid solutions/Ni2+,Ca2+Adulterate BiF3Positive pole and preparation method |
| CN106876681A (en) * | 2017-03-25 | 2017-06-20 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction liquid phase synthesis C/Bi/BiF3Compound fluorination bismuth anode material for lithium-ion batteries and preparation method thereof |
| CN106848263A (en) * | 2017-03-25 | 2017-06-13 | 宁波吉电鑫新材料科技有限公司 | A kind of continuous conduction liquid phase synthesis C/Ag, Bi/BiF3Compound fluorination bismuth anode material for lithium-ion batteries and preparation method thereof |
| CN110833802A (en) * | 2018-08-15 | 2020-02-25 | 漯河医学高等专科学校 | Method for preparing magnetic starch microspheres by gamma-ray irradiation |
| CN109603775A (en) * | 2018-11-30 | 2019-04-12 | 武汉理工大学 | A kind of carrying metal ion polyacrylamide magnetic bead and its preparation method and application |
| CN110721644A (en) * | 2019-10-22 | 2020-01-24 | 北京理工大学 | Radiation preparation method of vinyl polymer microcapsule |
| CN113861469A (en) * | 2021-10-19 | 2021-12-31 | 中国工程物理研究院激光聚变研究中心 | Preparation method of superparamagnetic polyimide composite film |
| CN113861469B (en) * | 2021-10-19 | 2023-10-17 | 中国工程物理研究院激光聚变研究中心 | Preparation method of superparamagnetism polyimide composite film |
| CN116764634A (en) * | 2022-03-11 | 2023-09-19 | 大庆油田有限责任公司 | Ionizing radiation catalyst, polyacrylamide solution and viscosity reduction method for polymer-containing sewage in oil field |
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