CN102627718A - Preparation method for crosslinked polystyrene microspheres of 10-100 microns - Google Patents
Preparation method for crosslinked polystyrene microspheres of 10-100 microns Download PDFInfo
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- CN102627718A CN102627718A CN2012100839667A CN201210083966A CN102627718A CN 102627718 A CN102627718 A CN 102627718A CN 2012100839667 A CN2012100839667 A CN 2012100839667A CN 201210083966 A CN201210083966 A CN 201210083966A CN 102627718 A CN102627718 A CN 102627718A
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Abstract
The invention relates to a preparation method for crosslinked polystyrene microspheres of 10-100 microns, and belongs to the field of high molecular microsphere materials. The preparation method comprises the steps as follows: firstly, dissolving a composite stabilizer in a water/ethanol mixed solvent by a method between a dispersion polymerization method and a suspension polymerization method; secondly, adding a mixed solution of an initiator, a monomer-styrene and a crosslinking agent-divinyl benzene; thirdly, heating a reaction system to the constant temperature, and polymerizing while stirring; and lastly, after the reaction is ended, filtering, washing and drying products to obtain the crosslinked polystyrene microspheres. The preparation method is simple, convenient and easy to operate, has simple steps and can prepare the crosslinked polystyrene microspheres of 10-100 microns through one step. The crosslinked polystyrene microspheres of 10-100 microns can be applied to the fields of chromatographic separation, biomedicine, coating and the like.
Description
Technical field
The present invention relates to a kind of method for preparing micron-level crosslinked polystyrene microsphere, belong to field of polymer microsphere materials.
Background technology
Announced that since Vanderhoff the micron order monodisperse polystyrene microsphere has all arrived widespread use in many scientific domains such as standard metering, information, analytical chemistry since the method for the highly homogeneous polystyrene microsphere of preparation.Micron-level crosslinked polystyrene microsphere has the specific surface area height, and crosslinking method and degree of crosslinking are controlled easily, and chemicalstability is good; By common solvent dissolving or swelling, mechanical strength is not high, and surface reaction activity is good; Hydrophobicity, biodegradable is ungood; The controllability of size of particles is good, is beneficial to advantages such as application and recovery, is the research focus of field of polymer microsphere materials.
Suspension polymerization, dispersion copolymerization method are the traditional methods of preparation micron order polystyrene microsphere; But the microspherulite diameter of suspension polymerization preparation is generally between 100 μ m ~ 1mm; And the microspherulite diameter of dispersion polymerization preparation is between 1 μ m ~ 10 μ m; And the microballoon that is between 10 ~ 100 μ m is difficult to obtain, and particularly will make microspherulite diameter is very difficult at the crosslinked polystyrene microsphere of 30 ~ 50 μ m.Therefore it is very necessary to seek a kind of method preparation 10 ~ 100 μ m microballoons that are between suspension polymerization and the dispersion polymerization.
Summary of the invention
The objective of the invention is to remedy the deficiency of prior art, a kind of method of preparation 10 ~ 100 μ m micron-level crosslinked polystyrene microspheres is provided.
The object of the invention is realized through following technical scheme: stablizer is dissolved in water and the alcoholic acid mixed solution prepares dispersion medium, the initiator Diisopropyl azodicarboxylate is dissolved in the mixed solution of monomer styrene and linking agent Vinylstyrene, then it is joined in the dispersion medium; Logical nitrogen; Stirring heating, 60 ~ 80 ℃ of reactions, polymerisate is through spinning; Absolute ethanol washing is dried to constant weight.
Stablizer according to the invention is one or more in Z 150PH, Vltra tears, polyoxyethylene glycol, Vinylpyrrolidone polymer, hydroxypropylcellulose and the gelatin, and its quality is 1 ~ 7% of a monomer styrene total mass, preferred 2 ~ 5%;
Monomer styrene quality of the present invention is 10% ~ 30% of a dispersion medium volume;
The quality of linking agent Vinylstyrene of the present invention is 0.5 ~ 3% of a monomer styrene total mass, preferred 1 ~ 2%.
Initiator Diisopropyl azodicarboxylate quality of the present invention is 1 ~ 6% of a monomer styrene total mass, preferred 2 ~ 4%.
Preferred 65 ~ 70 ℃ of polymeric reaction temperature of the present invention.
Stirring velocity 200-600 of the present invention rev/min, preferred 400 ~ 500 rev/mins.
Compared with present technology the present invention has following advantage: it is solvent that the present invention adopts water and alcoholic acid mixing solutions; The polymerization that utilization is between suspension polymerization and the dispersion polymerization prepares micron-level crosslinked polystyrene microsphere; The preparation method who provides is simple and easy to do; Step is simple, and a step can prepare the micron-sized crosslinked polystyrene microsphere of 10 ~ 100 μ m.
Description of drawings
The microscope figure of the crosslinked polystyrene microsphere of Fig. 1: embodiment 1.
The microscope figure of the crosslinked polystyrene microsphere of Fig. 2: embodiment 2.
The microscope figure of the crosslinked polystyrene microsphere of Fig. 3: embodiment 3.
Embodiment
Specify the present invention below and provide several embodiment:
Embodiment 1
0.3g stablizer Vltra tears and polyoxyethylene glycol (two kinds of stablizer ratios are 1:1) are dissolved in (water/ethanol=30/20 in 50 milliliters of mixed solvents; V/v); Then 0.375 gram Diisopropyl azodicarboxylate is dissolved in the mixed solution of 10 gram vinylbenzene and 0.2 gram Vinylstyrene, mixed solution is joined in the dispersion medium, stirred logical nitrogen 20 minutes; Stirring velocity is 450 rev/mins, then reaction vessel is placed 65 ℃ of water-bath reactions 12 hours.Polymerisate is through spinning, and absolute ethanol washing is dried to constant weight.
Microsphere optical microscope figure such as Fig. 1.
Embodiment 2
0.5g stablizer Vinylpyrrolidone polymer and hydroxypropylcellulose (two kinds of stablizer ratios are 1:1) are dissolved in (water/ethanol=50/50 in 100 milliliters of mixed solvents; V/v); Then 0.5 gram Diisopropyl azodicarboxylate is dissolved in the mixed solution of 10 gram vinylbenzene and 0.1 gram Vinylstyrene, mixed solution is joined in the dispersion medium, stirred logical nitrogen 20 minutes; Stirring velocity is 250 rev/mins, then reaction vessel is placed 80 ℃ of water-bath reactions 12 hours.Polymerisate is through spinning, and absolute ethanol washing is dried to constant weight.
Microsphere optical microscope figure such as Fig. 2.
Embodiment 3
0.3g stablizer Z 150PH is dissolved in (water/ethanol=30/20 in 50 milliliters of mixed solvents; V/v); Then 0.375 gram Diisopropyl azodicarboxylate is dissolved in the mixed solution of 10 gram vinylbenzene and 0.2 gram Vinylstyrene, mixed solution is joined in the dispersion medium, stirred logical nitrogen 20 minutes; Stirring velocity is 500 rev/mins, then reaction vessel is placed 70 ℃ of water-bath reactions 6 hours.Polymerisate is through spinning, and absolute ethanol washing is dried to constant weight.
Microsphere optical microscope figure such as Fig. 3.
The micron-sized crosslinked polystyrene microsphere of 10 ~ 100 μ m that the present invention makes can be applicable to fields such as chromatographic separation, biomedicine, coating.
Claims (6)
1.10 the preparation method of～100 microns crosslinked polystyrene microspheres is characterized in that, realizes through following steps: (1) is dissolved into stablizer in water and the alcoholic acid mixed solution and prepares dispersion medium; (2) the initiator Diisopropyl azodicarboxylate is dissolved in the mixed solution of monomer styrene and linking agent Vinylstyrene, then it is joined in the dispersion medium, logical nitrogen; Stirring heating, 60-80 ℃ of reaction, polymerisate is through spinning; Absolute ethanol washing is dried to constant weight; Said stablizer is one or more in Z 150PH, Vltra tears, polyoxyethylene glycol, Vinylpyrrolidone polymer, hydroxypropylcellulose, the gelatin, and the stablizer quality is the 1-7% of monomer styrene total mass; The monomer styrene quality is the 10%-30% of dispersion medium volume; The quality of linking agent Vinylstyrene is the 0.5-3% of monomer styrene total mass; Initiator Diisopropyl azodicarboxylate quality is the 1-6% of monomer styrene total mass.
2. the preparation method of 10～100 microns crosslinked polystyrene microspheres as claimed in claim 1 is characterized in that, the stablizer quality is the 2-5% of monomer styrene total mass.
3. the preparation method of 10～100 microns crosslinked polystyrene microspheres as claimed in claim 1 is characterized in that, linking agent Vinylstyrene quality is the 1-2% of monomer styrene total mass.
4. the preparation method of 10～100 microns crosslinked polystyrene microspheres as claimed in claim 1 is characterized in that, initiator Diisopropyl azodicarboxylate quality is the 2-4% of monomer styrene total mass.
5. like the preparation method of one of them described 10～100 microns crosslinked polystyrene microsphere of claim 1-4, it is characterized in that the preferred 65-70 of polymeric reaction temperature ℃.
6. like the preparation method of one of them described 10～100 microns crosslinked polystyrene microsphere of claim 1-4, it is characterized in that stirring velocity 200-600 rev/min.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875719A (en) * | 2012-10-22 | 2013-01-16 | 郑州大学 | Preparation method of 10-micron to 100-micron chloromethylated crosslinked polystyrene microspheres |
| CN103524646A (en) * | 2013-11-06 | 2014-01-22 | 惠州市富济电子材料有限公司 | Preparation method of polystyrene and silica gel with high refractive index |
| CN103736996A (en) * | 2014-01-24 | 2014-04-23 | 云南大学 | Method for preparing porous conductive micron-wire/rod covered composite microsphere material |
| CN105131164A (en) * | 2015-09-18 | 2015-12-09 | 北京化工大学 | Method for preparing monodisperse polymeric microspheres adopting snowman-shaped, dumbbell-shaped, raspberry-shaped or core-shell structure through one-step dispersion polymerization |
| CN106482995A (en) * | 2016-10-14 | 2017-03-08 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating standard substance of automatic Particle Counter of Liquid and preparation method thereof |
| CN106478856A (en) * | 2016-10-14 | 2017-03-08 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating standard substance and its preparation and the valued methods of PM10 sickle |
| CN106893124A (en) * | 2017-03-13 | 2017-06-27 | 厦门大学 | It is a kind of that the method for Nano microsphere ordered arrangement and its application on composite membrane is prepared are induced by polymer crystallization |
| CN110128732A (en) * | 2019-06-05 | 2019-08-16 | 中广核拓普（四川）新材料有限公司 | A kind of wear-resisting toughened polyethylene protective cover material and preparation method thereof |
| CN111533839A (en) * | 2020-04-23 | 2020-08-14 | 山东上禾中创科技成果转化有限公司 | Preparation method of porous polymer microspheres |
| CN114230698A (en) * | 2022-01-18 | 2022-03-25 | 吉林大学 | Preparation method of 10-70 mu m monodisperse polystyrene microsphere |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875719A (en) * | 2012-10-22 | 2013-01-16 | 郑州大学 | Preparation method of 10-micron to 100-micron chloromethylated crosslinked polystyrene microspheres |
| CN103524646A (en) * | 2013-11-06 | 2014-01-22 | 惠州市富济电子材料有限公司 | Preparation method of polystyrene and silica gel with high refractive index |
| CN103524646B (en) * | 2013-11-06 | 2016-06-01 | 惠州市富济电子材料有限公司 | The preparation method of a kind of high refractive index polystyrene and a kind of high refractive index silica gel |
| CN103736996A (en) * | 2014-01-24 | 2014-04-23 | 云南大学 | Method for preparing porous conductive micron-wire/rod covered composite microsphere material |
| CN103736996B (en) * | 2014-01-24 | 2016-03-30 | 云南大学 | A kind of method being covered with the composite microsphere material of conductive submicron line/rod preparing porous |
| CN105131164A (en) * | 2015-09-18 | 2015-12-09 | 北京化工大学 | Method for preparing monodisperse polymeric microspheres adopting snowman-shaped, dumbbell-shaped, raspberry-shaped or core-shell structure through one-step dispersion polymerization |
| CN106482995A (en) * | 2016-10-14 | 2017-03-08 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating standard substance of automatic Particle Counter of Liquid and preparation method thereof |
| CN106478856A (en) * | 2016-10-14 | 2017-03-08 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating standard substance and its preparation and the valued methods of PM10 sickle |
| CN106893124A (en) * | 2017-03-13 | 2017-06-27 | 厦门大学 | It is a kind of that the method for Nano microsphere ordered arrangement and its application on composite membrane is prepared are induced by polymer crystallization |
| CN106893124B (en) * | 2017-03-13 | 2019-07-30 | 厦门大学 | It is a kind of by polymer crystallization induce nanosphere ordered arrangement method and its in the application prepared on composite membrane |
| CN110128732A (en) * | 2019-06-05 | 2019-08-16 | 中广核拓普（四川）新材料有限公司 | A kind of wear-resisting toughened polyethylene protective cover material and preparation method thereof |
| CN111533839A (en) * | 2020-04-23 | 2020-08-14 | 山东上禾中创科技成果转化有限公司 | Preparation method of porous polymer microspheres |
| CN114230698A (en) * | 2022-01-18 | 2022-03-25 | 吉林大学 | Preparation method of 10-70 mu m monodisperse polystyrene microsphere |
| CN114230698B (en) * | 2022-01-18 | 2023-12-12 | 吉林大学 | Preparation method of 10-70 mu m monodisperse polystyrene microspheres |
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Application publication date: 20120808 |