CN101816909A - Preparation method of poly(phenylethylene-acrylic acid) magnetic polymer microsphere - Google Patents
Preparation method of poly(phenylethylene-acrylic acid) magnetic polymer microsphere Download PDFInfo
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- CN101816909A CN101816909A CN200910021903A CN200910021903A CN101816909A CN 101816909 A CN101816909 A CN 101816909A CN 200910021903 A CN200910021903 A CN 200910021903A CN 200910021903 A CN200910021903 A CN 200910021903A CN 101816909 A CN101816909 A CN 101816909A
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Abstract
The invention discloses a preparation method of poly(phenylethylene-acrylic acid) magnetic polymer microsphere, which comprises the steps: at first, preparing nano Fe3O4 water-based magnetic fluid with 10% of the solid content; based on unit weight, weighing and dissolving 6-12 parts of dispersion stabilizer in 1000 parts of mixed solution of absolute ethyl alcohol and water, adding 1-4 parts of initiator, 1-4 parts of crosslinking agent, 100 parts of phenylethylene, 10-30 parts of acrylic acid and 10-40 parts of Fe3O4 water-based magnetic fluid, and evenly stirring and subsequently implementing polyreaction for 10 hours at 65 DEG C. after the resultant product is subject to magnetic separation, immersion, pump filtration, washing and vacuum drying, the brown poly(phenylethylene-acrylic acid) magnetic polymer microsphere is obtained.
Description
Technical field
The present invention relates to the preparation method of high-molecular copolymer based nano composite material, specifically is the preparation of poly-(styrene-propene acid) magnetic macromolecular microsphere.
Background technology
Magnetic macromolecular microsphere is meant by suitable method and makes organic polymer and inorganic magnetic particle (particle diameter is in 10～30 nanometers) combine the microballoon of certain magnetic of having of formation and special construction.All have wide practical use in cell separation, immobilised enzymes, immunoassays, targeted drug, DNA (DNA) separation and nucleic acid hybridization, Chemical Decomposition and analysis, organic and biochemical synthetic, environment/fields such as food microorganisms detection.Chinese patent of the prior art all only relates to a kind of simple macromolecular material, does not relate to two kinds of macromolecular materials by binary copolymerization parcel inorganic magnetic particle, forms magnetic macromolecular microsphere.
Summary of the invention
The preparation method who the purpose of this invention is to provide poly-(styrene-propene acid) magnetic macromolecular microsphere.Be the preparation process of magnetic macromolecular microsphere below.
The present invention is the preparation method of poly-(styrene-propene acid) magnetic macromolecular microsphere, the steps include:
(1) adopt chemical coprecipitation to prepare nanometer Fe
3O
4, adopting and preparing solid content after poly ethyldiol modified is 10% nanometer Fe
3O
4Water-based magnetic fluid;
(2) press Unit Weight, prepare 1～4 part of initator, 1～4 part of crosslinking agent, be dissolved in 100 parts of styrene and 10～30 parts of acrylic acid nanometer Fe that the rear adding that stirs prepares
3O
4Water-based magnetic fluid adopts ultrasonic wave to disperse 5 minutes, is positioned over after the sealing and leaves standstill 24 hours in the refrigerator;
(3) take by weighing 6～12 parts dispersion stabilizer polyvinylpyrrolidone and be dissolved in the mixed solvent of 1000 parts absolute ethyl alcohol and water, the back that stirs moves into and has in the there-necked flask of thermometer, agitator and condenser pipe;
(4) when the solution in (3) is warming up to polymerization temperature, what add (2) step fast leaves standstill the solution that stirred in 24 hours;
(5) keeping mixing speed is that 150r/min, reaction temperature are 70 ℃, and polymerisation promptly obtained polymerizate in 10 hours;
(6) the product utilization kicker magnet that obtains being carried out magnetic separates;
(7) HCl of isolated magnetic macromolecular microsphere with 1mol/l soaked 48 hours, remove not wrapped nanometer Fe
3O
4
(8) magnetic macromolecular microsphere after will soaking carry out suction filtration, and with absolute ethyl alcohol and distilled water cross washing 8 times repeatedly;
(9) wash the back 50 ℃ of following vacuum drying 24 hours, promptly obtained brown poly-(styrene-propene acid) magnetic macromolecular microsphere.
The present invention is raw material with styrene and the acrylic monomers of technical grade, Fe
3O
4Be homemade nanometer Fe
3O
4Water-based magnetic fluid.
Poly-(styrene-propene acid) magnetic macromolecular microsphere of preparation raw material, by the Unit Weight umber be: 100 parts of styrene monomers, 10～30 parts in acrylic acid, 1～4 part of crosslinking agent.When the acrylic acid consumption is higher than 30 parts, can not form magnetic macromolecular microsphere; When the acrylic acid consumption was lower than 10 parts, magnetic macromolecular microsphere surface carboxyl-content was excessively low.When dosage of crosslinking agent surpassed 4 parts, product is bonded to piece can not form poly-(Styrene And Chloroalkyl Acrylates) magnetic macromolecular microsphere; When content is lower than 1 part, then do not have the stability that corresponding crosslinked action can not improve microballoon.
Initator of the present invention is oil-soluble initiators such as azodiisobutyronitrile or benzoyl peroxide.
The decentralized medium that the present invention adopts requires can dissolved monomer, initator, dispersion stabilizer, can not dissolve the polymer of generation again, and its composition is the mixed solution of water and absolute ethyl alcohol.
To prepare used stir speed (S.S.) be 150r/min to poly-(Styrene And Chloroalkyl Acrylates) magnetic macromolecular microsphere among the present invention.When mixing speed is too fast, with destroying the stereoscopic stable effect of dispersion stabilizer, not only can cause primary nuclei inhomogeneous, and can cause mutually reuniting between the later stage magnetic microsphere, have influence on generation and the growth course of magnetic microsphere; Mixing speed is crossed when slow, can produce cohesion, also is unfavorable for the generation of magnetic microsphere.
The specific embodiment
Be exemplifying embodiment more specifically below:
Embodiment 1:
(1) adopt chemical coprecipitation to prepare nanometer Fe
3O
4, adopting and preparing solid content after poly ethyldiol modified is 10% nanometer Fe
3O
4Water-based magnetic fluid;
(2) press Unit Weight, prepare 0.009kg initator azodiisobutyronitrile, 0.012kg crosslinking agent N, be dissolved into 0.6L styrene and 0.1L acrylic acid, the Fe of the rear adding 0.3L that stirs
3O
4Water-based magnetic fluid (solid content 10%) adopts ultrasonic wave to disperse 5 minutes, is positioned over after the sealing and leaves standstill 24 hours in the refrigerator;
(3) take by weighing 0.054kg dispersion stabilizer polyvinylpyrrolidone and be dissolved in the mixed solvent of the absolute ethyl alcohol of 7.5L and 2.5L water, the back that stirs moves into and has in the there-necked flask of thermometer, agitator and condenser pipe;
(4) when the solution in (3) step is warming up to polymerization temperature, what add (2) step fast leaves standstill the solution that stirred in 24 hours;
(5) keeping mixing speed is that 150r/min, reaction temperature are 70 ℃, and polymerisation promptly obtained polymerizate in 8 hours;
(6) the product utilization kicker magnet that obtains being carried out magnetic separates;
(7) HCl of isolated magnetic macromolecular microsphere with 1mol/l soaked 48 hours, remove not wrapped nanometer Fe
3O
4
(8) magnetic macromolecular microsphere after will soaking carry out suction filtration, and with absolute ethyl alcohol and distilled water cross washing 8 times repeatedly;
(9) wash the back 50 ℃ of following vacuum drying 24 hours, promptly obtained brown poly-(styrene-propene acid) magnetic macromolecular microsphere.
Embodiment 2:
(1) adopt chemical coprecipitation to prepare nanometer Fe
3O
4, adopting and preparing solid content after poly ethyldiol modified is 10% nanometer Fe
3O
4Water-based magnetic fluid;
(2) press Unit Weight, prepare 0.018kg initator azodiisobutyronitrile, 0.022kg crosslinking agent N, be dissolved into 1.0L styrene and 0.3L acrylic acid, the Fe of the rear adding 0.5L that stirs
3O
4Water-based magnetic fluid (solid content 10%) adopts ultrasonic wave to disperse 5 minutes, is positioned over after the sealing and leaves standstill 24 hours in the refrigerator;
(3) take by weighing 0.073kg dispersion stabilizer polyvinylpyrrolidone and be dissolved in the mixed solvent of the absolute ethyl alcohol of 8.0L and 2.0L water, the back that stirs moves into and has in the there-necked flask of thermometer, agitator and condenser pipe;
(4) when the solution in (3) step is warming up to polymerization temperature, what add (2) step fast leaves standstill the solution that stirred in 24 hours;
(5) keeping mixing speed is that 150r/min, reaction temperature are 70 ℃, and polymerisation promptly obtained polymerizate in 10 hours;
(6) the product utilization kicker magnet that obtains being carried out magnetic separates;
(7) HCl of isolated magnetic macromolecular microsphere with 1mol/l soaked 48 hours, remove not wrapped nanometer Fe
3O
4
(8) magnetic macromolecular microsphere after will soaking carry out suction filtration, and with absolute ethyl alcohol and distilled water cross washing 8 times repeatedly;
(9) wash the back 50 ℃ of following vacuum drying 24 hours, promptly obtained brown poly-(styrene-propene acid) magnetic macromolecular microsphere.
Embodiment 3:
(1) adopt chemical coprecipitation to prepare nanometer Fe
3O
4, adopting and preparing solid content after poly ethyldiol modified is 10% nanometer Fe
3O
4Water-based magnetic fluid;
(2) press Unit Weight, prepare 0.027 initator azodiisobutyronitrile, 0.045kg crosslinking agent N, be dissolved into 1.0L styrene and 0.2L acrylic acid, the Fe of the rear adding 0.7L that stirs
3O
4Water-based magnetic fluid (solid content 10%) adopts ultrasonic wave to disperse 5 minutes, is positioned over after the sealing and leaves standstill 24 hours in the refrigerator;
(3) take by weighing 0.109kg kg dispersion stabilizer polyvinylpyrrolidone and be dissolved in the mixed solvent of the absolute ethyl alcohol of 8.5L and 1.5L water, the back that stirs moves into and has in the there-necked flask of thermometer, agitator and condenser pipe;
(4) when the solution in (3) step is warming up to polymerization temperature, what add (2) step fast leaves standstill the solution that stirred in 24 hours;
(5) keeping mixing speed is that 150r/min, reaction temperature are 65 ℃, and polymerisation promptly obtained polymerizate in 10 hours;
(6) the product utilization kicker magnet that obtains being carried out magnetic separates;
(7) HCl of isolated magnetic macromolecular microsphere with 1mol/l soaked 48 hours, remove not wrapped nanometer Fe
3O
4
(8) magnetic macromolecular microsphere after will soaking carry out suction filtration, and with absolute ethyl alcohol and distilled water cross washing 8 times repeatedly;
(9) wash the back 50 ℃ of following vacuum drying 24 hours, promptly obtained brown poly-(styrene-propene acid) magnetic macromolecular microsphere.
Embodiment 4:
(1) adopt chemical coprecipitation to prepare nanometer Fe
3O
4, adopting and preparing solid content after poly ethyldiol modified is 10% nanometer Fe
3O
4Water-based magnetic fluid;
(2) press Unit Weight, prepare 0.027 initator azodiisobutyronitrile, 0.034kg crosslinking agent N, be dissolved into 0.8L styrene and 0.2L acrylic acid, the Fe of the rear adding 0.5L that stirs
3O
4Water-based magnetic fluid (solid content 10%) adopts ultrasonic wave to disperse 5 minutes, is positioned over after the sealing and leaves standstill 24 hours in the refrigerator;
(3) take by weighing 0.091kg kg dispersion stabilizer polyvinylpyrrolidone and be dissolved in the mixed solvent of the absolute ethyl alcohol of 9.0L and 1.0L water, the back that stirs moves into and has in the there-necked flask of thermometer, agitator and condenser pipe;
(4) when the solution in (3) step is warming up to polymerization temperature, what add (2) step fast leaves standstill the solution that stirred in 24 hours;
(5) keeping mixing speed is that 150r/min, reaction temperature are 75 ℃, and polymerisation promptly obtained polymerizate in 10 hours;
(6) the product utilization kicker magnet that obtains being carried out magnetic separates;
(7) HCl of isolated magnetic macromolecular microsphere with 1mol/l soaked 48 hours, remove not wrapped nanometer Fe
3O
4
(8) magnetic macromolecular microsphere after will soaking carry out suction filtration, and with absolute ethyl alcohol and distilled water cross washing 8 times repeatedly;
(9) wash the back 50 ℃ of following vacuum drying 24 hours, promptly obtained brown poly-(styrene-propene acid) magnetic macromolecular microsphere.
Claims (1)
1. the preparation method of poly-(styrene-propene acid) magnetic macromolecular microsphere the steps include:
(1) adopt chemical coprecipitation to prepare nanometer Fe
3O
4, adopting and preparing solid content after poly ethyldiol modified is 10% nanometer Fe
3O
4Water-based magnetic fluid;
(2) press Unit Weight, prepare 1～4 part of initator, 1～4 part of crosslinking agent, be dissolved in 100 parts of styrene and 10～30 parts of acrylic acid nanometer Fe that the rear adding that stirs prepares
3O
4Water-based magnetic fluid adopts ultrasonic wave to disperse 5 minutes, is positioned over after the sealing and leaves standstill 24 hours in the refrigerator;
(3) take by weighing 6～12 parts dispersion stabilizer polyvinylpyrrolidone and be dissolved in the mixed solvent of 1000 parts absolute ethyl alcohol and water, the back that stirs moves into and has in the there-necked flask of thermometer, agitator and condenser pipe;
(4) when the solution in (3) step is warming up to polymerization temperature, what add (2) step fast leaves standstill the solution that stirred in 24 hours;
(5) keeping mixing speed is that 150r/min, reaction temperature are 65～75 ℃, and polymerisation promptly obtained polymerizate in 8～10 hours;
(6) the product utilization kicker magnet that obtains being carried out magnetic separates;
(7) HCl of isolated magnetic macromolecular microsphere with 1mol/l soaked 48 hours, remove not wrapped nanometer Fe
3O
4
(8) magnetic macromolecular microsphere after will soaking carry out suction filtration, and with absolute ethyl alcohol and distilled water cross washing 8 times repeatedly;
(9) wash the back 50 ℃ of following vacuum drying 24 hours, promptly obtained brown poly-(styrene-propene acid) magnetic macromolecular microsphere.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304200A (en) * | 2011-05-27 | 2012-01-04 | 中国海洋石油总公司 | Crosslinked polymer microspheres and preparation method thereof |
| CN103041862A (en) * | 2012-12-21 | 2013-04-17 | 厦门大学 | Nano-vanadium composite catalytic material capable of being magnetically separated and preparation method thereof |
| CN103694392A (en) * | 2013-12-09 | 2014-04-02 | 中北大学 | Method for preparing carboxyl polystyrene copolymerized fluorescent microsphere |
| CN104492397A (en) * | 2014-12-11 | 2015-04-08 | 上海烟草集团有限责任公司 | Carboxyl polystyrene magnetic microspherical composite material for reducing ammonia release in smoke of cigarette and preparation method and application of carboxyl polystyrene magnetic microspherical composite material |
| CN109759029A (en) * | 2019-02-22 | 2019-05-17 | 合众（佛山）化工有限公司 | A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent and preparation method thereof |
| CN110787743A (en) * | 2019-10-25 | 2020-02-14 | 西南民族大学 | Magnetic-response photonic crystal, and simple large-scale preparation method and application thereof |
| CN111229178A (en) * | 2020-02-11 | 2020-06-05 | 南通大学 | Poly- (methacrylic acid-ethylene glycol diacrylate) @ Fe3O4Water treatment agent and preparation method thereof |
-
2009
- 2009-03-20 CN CN200910021903A patent/CN101816909A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304200A (en) * | 2011-05-27 | 2012-01-04 | 中国海洋石油总公司 | Crosslinked polymer microspheres and preparation method thereof |
| CN102304200B (en) * | 2011-05-27 | 2013-08-21 | 中国海洋石油总公司 | Crosslinked polymer microspheres and preparation method thereof |
| CN103041862A (en) * | 2012-12-21 | 2013-04-17 | 厦门大学 | Nano-vanadium composite catalytic material capable of being magnetically separated and preparation method thereof |
| CN103694392A (en) * | 2013-12-09 | 2014-04-02 | 中北大学 | Method for preparing carboxyl polystyrene copolymerized fluorescent microsphere |
| CN104492397A (en) * | 2014-12-11 | 2015-04-08 | 上海烟草集团有限责任公司 | Carboxyl polystyrene magnetic microspherical composite material for reducing ammonia release in smoke of cigarette and preparation method and application of carboxyl polystyrene magnetic microspherical composite material |
| CN109759029A (en) * | 2019-02-22 | 2019-05-17 | 合众（佛山）化工有限公司 | A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent and preparation method thereof |
| CN110787743A (en) * | 2019-10-25 | 2020-02-14 | 西南民族大学 | Magnetic-response photonic crystal, and simple large-scale preparation method and application thereof |
| CN111229178A (en) * | 2020-02-11 | 2020-06-05 | 南通大学 | Poly- (methacrylic acid-ethylene glycol diacrylate) @ Fe3O4Water treatment agent and preparation method thereof |
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Open date: 20100901 |