CN104558316A - Method for synthesizing polystyrene microspheres based on emulsion method - Google Patents
Method for synthesizing polystyrene microspheres based on emulsion method Download PDFInfo
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Abstract
The invention discloses a method for synthesizing polystyrene microspheres based on an emulsion method. The method comprises the following steps: by taking lauryl sodium sulfate as an emulsifier, PVP as a dispersing agent, V-50 as an initiator and styrene as a monomer, synthesizing polystyrene nanometer microspheres by adopting an emulsion polymerization method; and stirring under a nitrogen atmosphere for 0.5 hour so as to form emulsion, heating to 40 DEG C, adding 0.12g of V-50 to drive polymerization, reacting at the temperature of 60 DEG C, performing reflux condensation, and polymerizing under nitrogen conditions for 24 hours. According to the method for synthesizing polystyrene microspheres based on the emulsion method provided by the invention, the process is simple, the conversion rate of styrene under the optimized condition is 98 percent, and the molecular weight of polystyrene is 320000.
Description
Technical field
The invention discloses based on emulsion method polystyrene microsphere synthetic method.
Background technology
Polymer microballoon has that specific surface area is large, high adsorption capacity, cohesion large and the characteristic such as surface reaction ability is strong.Even-grained polymer microballoon, of many uses as functional high molecule material, thus its research more and more draws attention.Polystyrene microsphere has wide practical use in synthesis large pore molecular sieve, adopts water-oil ratio to be 100:3 in polystyrene microsphere synthesis in the past, thus obtained microsphere particle diameter comparatively large (>100nm).
Summary of the invention
The present invention is based on emulsion method polystyrene microsphere synthetic method, the method adopts sodium lauryl sulphate to be emulsifying agent, PVP is adopted to be monomer as dispersion agent, V-50 as initiator, vinylbenzene, under the condition of low water-oil ratio, adopt emulsion polymerisation process to synthesize Properties of Polystyrene Nano Particles, stir 0.5h under nitrogen atmosphere and form emulsion, be warming up to 40 DEG C, then the V-50 adding 0.12g drives polymerization, reacts at 60 degrees Celsius, is polymerized 24h under reflux condensation mode, condition of nitrogen gas.
The method adopts following steps:
(1) preparation of polystyrene (PSt) Nano microsphere;
100mL water and sodium lauryl sulphate is added in there-necked flask, under the condition of low water-oil ratio, emulsion polymerisation process is adopted to synthesize Properties of Polystyrene Nano Particles, stir 0.5h under nitrogen atmosphere and form emulsion, be warming up to 40 DEG C, then the V-50 adding 0.12g drives polymerization, reaction is at 60 degrees Celsius, 24h is polymerized under reflux condensation mode, condition of nitrogen gas, stirring and dissolving is clarified to solution, after adding a certain amount of V-50 and vinylbenzene emulsification certain hour again, drip the aqueous solution (dripping off in 1h) of a certain amount of ammonium persulphate, isothermal reaction certain hour;
(2) breakdown of emulsion;
Emulsion at room temperature stirred, drip calcium chloride water, with distilled water diluting, vacuum filtration, with distilled water repeated washing suction filtration 3 times, then use washing with alcohol suction filtration 3 times, dry, be placed in 24h in 90 DEG C of baking ovens, drying obtains white products;
(3) sign of polystyrene polymeric microballoon;
By the sucking-off of nattier blue polystyrene polymeric microballoon dispersion liquid dropper, instillation 50mL small beaker one, with distilled water diluting 30 times, vibrator is adjusted to 100 speed oscillation 2.5h, until clarification, then drips on the cover slip, Air drying.Measure with electron-microscope scanning, need metal spraying process before measurement, scanning electron microscope operating voltage 1.00kV.
The particle diameter of described high-polystyrene and molecular weight temperature be less than 65 DEG C.
Described PVP is less than 40 DEG C as dispersion agent, V-50 as initiator is temperature required.
Described water-oil ratio is under the condition of low water-oil ratio 100:30, synthesizes monomolecular polystyrene microsphere.
The positively effect that the present invention has is:
The present invention is based on emulsion method polystyrene microsphere synthetic method craft simple, cinnamic transformation efficiency reaches 98% in optimal conditions, the molecular weight of polystyrene reaches 320,000.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and be not used in restriction invention.
Based on emulsion method polystyrene microsphere synthetic method.The method adopts sodium lauryl sulphate to be emulsifying agent, PVP is adopted to be monomer as dispersion agent, V-50 as initiator, vinylbenzene, under the condition of low water-oil ratio, emulsion polymerisation process is adopted to synthesize Properties of Polystyrene Nano Particles, stir 0.5h under nitrogen atmosphere and form emulsion, be warming up to 40 DEG C, the V-50 then adding 0.12g drives polymerization, reaction, at 60 degrees Celsius, is polymerized 24h under reflux condensation mode, condition of nitrogen gas.
The method adopts following steps:
(1) preparation of polystyrene (PSt) Nano microsphere;
100mL water and sodium lauryl sulphate is added in there-necked flask, under the condition of low water-oil ratio, emulsion polymerisation process is adopted to synthesize Properties of Polystyrene Nano Particles, stir 0.5h under nitrogen atmosphere and form emulsion, be warming up to 40 DEG C, then the V-50 adding 0.12g drives polymerization, reaction is at 60 degrees Celsius, 24h is polymerized under reflux condensation mode, condition of nitrogen gas, stirring and dissolving is clarified to solution, after adding a certain amount of V-50 and vinylbenzene emulsification certain hour again, drip the aqueous solution (dripping off in 1h) of a certain amount of ammonium persulphate, isothermal reaction certain hour;
(2) breakdown of emulsion;
Emulsion at room temperature stirred, drip calcium chloride water, with distilled water diluting, vacuum filtration, with distilled water repeated washing suction filtration 3 times, then use washing with alcohol suction filtration 3 times, dry, be placed in 24h in 90 DEG C of baking ovens, drying obtains white products;
(4) sign of polystyrene polymeric microballoon;
By the sucking-off of nattier blue polystyrene polymeric microballoon dispersion liquid dropper, instillation 50mL small beaker one, with distilled water diluting 30 times, vibrator is adjusted to 100 speed oscillation 2.5h, until clarification, then drips on the cover slip, Air drying.Measure with electron-microscope scanning, need metal spraying process before measurement, scanning electron microscope operating voltage 1.00kV.
The particle diameter of high-polystyrene and molecular weight temperature be less than 65 DEG C.
PVP is less than 40 DEG C as dispersion agent, V-50 as initiator is temperature required.
Water-oil ratio is under the condition of low water-oil ratio 100:30, synthesizes monomolecular polystyrene microsphere.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. based on emulsion method polystyrene microsphere synthetic method, it is characterized in that: the method adopts following steps: the preparation of (1) polystyrene (PSt) Nano microsphere; 100mL water and sodium lauryl sulphate is added in there-necked flask, under the condition of low water-oil ratio, emulsion polymerisation process is adopted to synthesize Properties of Polystyrene Nano Particles, stir 0.5h under nitrogen atmosphere and form emulsion, be warming up to 40 DEG C, then the V-50 adding 0.12g drives polymerization, reaction is at 60 degrees Celsius, 24h is polymerized under reflux condensation mode, condition of nitrogen gas, stirring and dissolving is clarified to solution, after adding a certain amount of V-50 and vinylbenzene emulsification certain hour again, drip the aqueous solution (dripping off in 1h) of a certain amount of ammonium persulphate, isothermal reaction certain hour; (2) breakdown of emulsion; Emulsion at room temperature stirred, drip calcium chloride water, with distilled water diluting, vacuum filtration, with distilled water repeated washing suction filtration 3 times, then use washing with alcohol suction filtration 3 times, dry, be placed in 24h in 90 DEG C of baking ovens, drying obtains white products;
The sign of polystyrene polymeric microballoon; By the sucking-off of nattier blue polystyrene polymeric microballoon dispersion liquid dropper, instillation 50mL small beaker one, with distilled water diluting 30 times, vibrator is adjusted to 100 speed oscillation 2.5h, until clarification, then drips on the cover slip, Air drying, measure with electron-microscope scanning, need metal spraying process before measurement, scanning electron microscope operating voltage 1.00kV.
2., according to claim 1 based on emulsion method polystyrene microsphere synthetic method, it is characterized in that, the particle diameter of described high-polystyrene and molecular weight temperature be less than 65 DEG C.
3. according to claim 1 based on emulsion method polystyrene microsphere synthetic method, it is characterized in that, described PVP is less than 40 DEG C as dispersion agent, V-50 as initiator is temperature required.
4. according to claim 1 based on emulsion method polystyrene microsphere synthetic method, it is characterized in that, described water-oil ratio is under the condition of low water-oil ratio 100:30, synthesizes monomolecular polystyrene microsphere.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105384856A (en) * | 2015-12-10 | 2016-03-09 | 重庆三零三科技有限公司 | Preparation method of polystyrene microsphere |
| CN107936167A (en) * | 2017-12-21 | 2018-04-20 | 苏州希尔盖森新材料有限公司 | One kind has hydrophilic polystyrene microsphere |
| CN109659570A (en) * | 2019-01-09 | 2019-04-19 | 长江大学 | The application of the metal organic framework compound hollow microsphere of load iron cobalt sulfide |
| CN109728311A (en) * | 2019-01-09 | 2019-05-07 | 长江大学 | The metal organic framework compound hollow microsphere of load iron cobalt sulfide |
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| CN103387681A (en) * | 2012-05-07 | 2013-11-13 | 中国石油化工股份有限公司 | Preparation method and application of polystyrene plastic pellet |
| CN103333280A (en) * | 2013-06-17 | 2013-10-02 | 厦门大学 | Method for regulating monodispersity of polystyrene microsphere based on hydrothermal treatment |
| CN103709431A (en) * | 2013-12-18 | 2014-04-09 | 镇江森华阻燃工程科技有限公司 | Polystyrene with high flame retardant property and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384856A (en) * | 2015-12-10 | 2016-03-09 | 重庆三零三科技有限公司 | Preparation method of polystyrene microsphere |
| CN107936167A (en) * | 2017-12-21 | 2018-04-20 | 苏州希尔盖森新材料有限公司 | One kind has hydrophilic polystyrene microsphere |
| CN109659570A (en) * | 2019-01-09 | 2019-04-19 | 长江大学 | The application of the metal organic framework compound hollow microsphere of load iron cobalt sulfide |
| CN109728311A (en) * | 2019-01-09 | 2019-05-07 | 长江大学 | The metal organic framework compound hollow microsphere of load iron cobalt sulfide |
| CN109728311B (en) * | 2019-01-09 | 2021-08-10 | 长江大学 | Metal organic framework compound hollow microsphere loaded with iron cobalt sulfide |
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