CN101817902A - Method for preparing micron-level crosslinked polystyrene microsphere - Google Patents
Method for preparing micron-level crosslinked polystyrene microsphere Download PDFInfo
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- CN101817902A CN101817902A CN201010111266A CN201010111266A CN101817902A CN 101817902 A CN101817902 A CN 101817902A CN 201010111266 A CN201010111266 A CN 201010111266A CN 201010111266 A CN201010111266 A CN 201010111266A CN 101817902 A CN101817902 A CN 101817902A
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- polystyrene microsphere
- crosslinked polystyrene
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Abstract
The invention discloses a method for preparing a micron-level crosslinked polystyrene microsphere. The method is characterized by comprising the following steps of: dissolving a styrene monomer, pentaerythritol tetra-acrylate serving as a crosslinking agent and azodiisobutyronitrile serving as an evocating agent in ethanol which is an environmentally-friendly solvent, vibrating at the constant temperature for reaction, performing centrifugal separation on polymerisate, washing the polymerisate with absolute ethanol, and drying to constant weight. Through the preparation method disclosed by the invention, the crosslinked polystyrene microsphere with good single dispersion and particle diameter range between 0.3 and 1 micron can be obtained and can be applied to the fields of biological medicament, chromatographic packing, chemical analysis 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
Along with science and technology development, polymeric microball material in the application in fields such as standard metering, medical immunology, biotechnology, analytical chemistry, information, chemical industry and microelectronics more and more widely.Micron-level crosslinked polystyrene microsphere has the specific surface area height, the mechanical strength height, surface reaction activity is good, hydrophobicity, biodegradable is ungood, the controllability of size of particles is good, not dissolved or swelling by common solvent, be beneficial to advantages such as application and recovery, is the research focus of field of polymer microsphere materials.
Suspension polymerization, emulsion polymerization and dispersion copolymerization method are the traditional methods of preparation polystyrene microsphere, but these methods all need to add stablizer or emulsifying agent in reaction system.In recent years, precipitation polymerization method is because its reaction system is simple, emulsifier free or stablizer, and plurality of advantages such as plant and instrument is simple, and operational condition is easily controlled, and the pure and aftertreatment of product is easy extremely people is paid close attention to.In the precipitation polymerization method, solvent commonly used is an acetonitrile, but the toxicity of acetonitrile is big, and the exploitation of the novel dissolvent system of precipitation polymerization has caused people's very big concern, seek a kind of environmentally friendly solvent and replace acetonitrile, it is particularly important to solve the problem that acetonitrile toxicity is big in the precipitation polymerization method.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of method for preparing micron-level crosslinked polystyrene microsphere in environmentally friendly etoh solvent is provided.
Purpose of the present invention can reach by following measure: a kind of method for preparing micron-level crosslinked polystyrene microsphere, it is characterized in that: with monomer styrene, the linking agent tetramethylol methane tetraacrylate, the initiator Diisopropyl azodicarboxylate is dissolved in the ethanol, wherein, the consumption of vinylbenzene and tetramethylol methane tetraacrylate is 0.5～4% of a total ethanol volume, the consumption of tetramethylol methane tetraacrylate is 20～90% of a monomer cumulative volume, initiator amount is 0.5～8% of a monomer total mass, the vibration heating, at 65～78 degrees centigrade, under 30～110 rev/mins of oscillation frequency, the reaction times is not less than 1.5 hours, and polymerisate is through centrifugation, absolute ethanol washing is dried to constant weight.The volume fraction that the vinylbenzene among the present invention and the consumption of tetramethylol methane tetraacrylate account for the total ethanol volume preferably 1～2%.
The volume fraction that the consumption of the linking agent tetramethylol methane tetraacrylate among the present invention accounts for the monomer cumulative volume preferably 50～80%.
The massfraction that initiator amount among the present invention accounts for the monomer total mass preferably 1～3%.
Preferably 70～75 degrees centigrade of polymeric reaction temperatures among the present invention.
Preferably 50～90 rev/mins of oscillation frequency among the present invention.
Compared with the prior art the present invention has following advantage: the present invention adopts environmentally friendly etoh solvent to make solvent, utilize precipitation polymerization method to prepare micron-level crosslinked polystyrene microsphere, the preparation method who provides is simple and easy to do, do not need to add any emulsifying agent and stablizer in the reaction system, can obtain micron-level crosslinked polystyrene microsphere.
Embodiment
Describe the present invention below in detail and provide several embodiment:
Embodiment 1
With 50 milliliters of ethanol, 0.1 milliliter of vinylbenzene, 0.4 milliliter of tetramethylol methane tetraacrylate and Diisopropyl azodicarboxylate 0.0057 gram mix, 70 rev/mins of constant oscillation frequency, 70 degrees centigrade were reacted 4 hours.Polymerisate is through centrifugation, and absolute ethanol washing is dried to constant weight.
Gained polystyrene microsphere median size is 0.59 micron, and monodispersity is good.
Embodiment 2
With 50 milliliters of ethanol, 0.1 milliliter of vinylbenzene, 0.4 milliliter of tetramethylol methane tetraacrylate and Diisopropyl azodicarboxylate 0.0057 gram mix, 30 rev/mins of constant oscillation frequency, 70 degrees centigrade were reacted 4 hours.Polymerisate is through centrifugation, and absolute ethanol washing is dried to constant weight.
Gained polystyrene microsphere median size is 0.33 micron, and monodispersity is good.
Embodiment 3
With 50 milliliters of ethanol, 0.05 milliliter of vinylbenzene, 0.45 milliliter of tetramethylol methane tetraacrylate and Diisopropyl azodicarboxylate 0.0059 gram mix, 70 rev/mins of constant oscillation frequency, 70 degrees centigrade were reacted 4 hours.Polymerisate is through centrifugation, and absolute ethanol washing is dried to constant weight.
Gained polystyrene microsphere median size is 0.55 micron, and monodispersity is good.
Embodiment 4
With 50 milliliters of ethanol, 0.25 milliliter of vinylbenzene, 0.25 milliliter of tetramethylol methane tetraacrylate and Diisopropyl azodicarboxylate 0.0158 gram mix, 120 rev/mins of constant oscillation frequency, 70 degrees centigrade were reacted 4 hours.Polymerisate is through centrifugation, and absolute ethanol washing is dried to constant weight.
Gained polystyrene microsphere median size is 0.47 micron, and monodispersity is good.
Embodiment 5
With 50 milliliters of ethanol, 0.1 milliliter of vinylbenzene, 0.4 milliliter of tetramethylol methane tetraacrylate and Diisopropyl azodicarboxylate 0.0454 gram mix, 70 rev/mins of constant oscillation frequency, 70 degrees centigrade were reacted 4 hours.Polymerisate is through centrifugation, and absolute ethanol washing is dried to constant weight.
Gained polystyrene microsphere median size is 0.49 micron, and monodispersity is good.
Embodiment 6
With 50 milliliters of ethanol, 0.4 milliliter of vinylbenzene, 0.1 milliliter of tetramethylol methane tetraacrylate and Diisopropyl azodicarboxylate 0.0060 gram mix, 70 rev/mins of constant oscillation frequency, 75 degrees centigrade were reacted 1.5 hours.Polymerisate is through centrifugation, and absolute ethanol washing is dried to constant weight.
Gained polystyrene microsphere median size is 0.32 micron, and monodispersity is good.
Embodiment 7
With 50 milliliters of ethanol, 0.1 milliliter of vinylbenzene, 0.4 milliliter of tetramethylol methane tetraacrylate and Diisopropyl azodicarboxylate 0.0058 gram mix, 70 rev/mins of constant oscillation frequency, 70 degrees centigrade were reacted 10 hours.Polymerisate is through centrifugation, and absolute ethanol washing is dried to constant weight.
Gained polystyrene microsphere median size is 0.78 micron, and monodispersity is good.
Claims (6)
1. method for preparing micron-level crosslinked polystyrene microsphere, it is characterized in that: with monomer styrene, the linking agent tetramethylol methane tetraacrylate, the initiator Diisopropyl azodicarboxylate is dissolved in the ethanol, wherein, the consumption of vinylbenzene and tetramethylol methane tetraacrylate is 0.5～4% of an ethanol volume, the consumption of tetramethylol methane tetraacrylate is 20～90% of a monomer cumulative volume, and initiator amount is 0.5～8% of a monomer total mass, the vibration heating, polymeric reaction temperature is 65～78 degrees centigrade, oscillation frequency is 30～110 rev/mins, and the reaction times is not less than 1.5 hours, and polymerisate is through centrifugation, absolute ethanol washing is dried to constant weight.
2. a kind of method for preparing micron-level crosslinked polystyrene microsphere according to claim 1 is characterized in that: the consumption of described monomer styrene and linking agent tetramethylol methane tetraacrylate is 1～2% of an ethanol volume.
3. a kind of method for preparing micron-level crosslinked polystyrene microsphere according to claim 1 is characterized in that: the consumption of tetramethylol methane tetraacrylate is 50～80% of a monomer cumulative volume.
4. a kind of method for preparing micron-level crosslinked polystyrene microsphere according to claim 1 is characterized in that: initiator amount is 1～3% of a monomer total mass.
5. a kind of method for preparing micron-level crosslinked polystyrene microsphere according to claim 1 is characterized in that: polymeric reaction temperature is 70～75 degrees centigrade.
6. a kind of method for preparing micron-level crosslinked polystyrene microsphere according to claim 1 is characterized in that: oscillation frequency is 50～90 rev/mins.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101112665A CN101817902B (en) | 2010-01-22 | 2010-01-22 | Method for preparing micron-level crosslinked polystyrene microsphere |
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| CN2010101112665A CN101817902B (en) | 2010-01-22 | 2010-01-22 | Method for preparing micron-level crosslinked polystyrene microsphere |
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| CN101817902A true CN101817902A (en) | 2010-09-01 |
| CN101817902B CN101817902B (en) | 2011-11-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161738A (en) * | 2010-12-31 | 2011-08-24 | 浙江大学 | Method for preparing multiple environment-responsive hairy polymer microspheres by loading photoinitiator and reversible addition-fragmentation chain transfer (RAFT) reagent onto different spheres respectively |
| CN102898582A (en) * | 2011-07-26 | 2013-01-30 | 比亚迪股份有限公司 | Micron-sized polymer microsphere, and preparation method and light diffusion plate 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 |
| CN106478857A (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 airborne particle counter and preparation method thereof |
-
2010
- 2010-01-22 CN CN2010101112665A patent/CN101817902B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161738A (en) * | 2010-12-31 | 2011-08-24 | 浙江大学 | Method for preparing multiple environment-responsive hairy polymer microspheres by loading photoinitiator and reversible addition-fragmentation chain transfer (RAFT) reagent onto different spheres respectively |
| CN102898582A (en) * | 2011-07-26 | 2013-01-30 | 比亚迪股份有限公司 | Micron-sized polymer microsphere, and preparation method and light diffusion plate 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 |
| CN106478857A (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 airborne particle counter and preparation method thereof |
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| Publication number | Publication date |
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| CN101817902B (en) | 2011-11-23 |
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Assignee: Sk Industrial (Shantou) polystyrene resin Co. Ltd. Assignor: Ludong University Contract record no.: 2012440000398 Denomination of invention: Method for preparing micron-level crosslinked polystyrene microsphere Granted publication date: 20111123 License type: Exclusive License Open date: 20100901 Record date: 20120711 |
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Granted publication date: 20111123 Termination date: 20180122 |