CN103570849A - Method for preparing polystyrene nanosphere for novel suede-like conductive glass - Google Patents
Method for preparing polystyrene nanosphere for novel suede-like conductive glass Download PDFInfo
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- CN103570849A CN103570849A CN201310481710.6A CN201310481710A CN103570849A CN 103570849 A CN103570849 A CN 103570849A CN 201310481710 A CN201310481710 A CN 201310481710A CN 103570849 A CN103570849 A CN 103570849A
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Abstract
The invention discloses a method for preparing a polystyrene nanosphere for novel suede-like conductive glass. The method comprises the following steps of 1) purifying the raw materials; 2) synthesizing the polystyrene nanosphere, mixing processed styrene with ultrapure water in a four-neck flask; under the protection of nitrogen, heating up to 70-80 DEG C, and stirring for 30 minutes; then adding an initiator solution, reacting for 5-12 hours, wherein the concentration of styrene is 0.5-0.9mM and the concentration of the initiator is 1.8-2.8mM; and 3) treating the reacted polystyrene nanosphere. The prepared polystyrene nanosphere has uniform and controllable grain size, high density, and uniform film-forming, and well meets the application requirements of the novel suede-like conductive glass, and the preparation method is simple to operate, greatly shortens operation time, does not use special raw materials, does not pollute the environment, has low cost, and is applicable to large-scale preparation of the polystyrene nanosphere.
Description
Technical field
The present invention relates to macromolecule material preparation area, be specifically related to a kind of preparation method who is applied to the polystyrene nanospheres of novel matte conductive glass.
Background technology
Transparent conducting glass refers to that the one side on ordinary plate glass is coated with transparent conductive film, thereby makes whole glass have specific glass transparent and conduction dual property.Transparent conducting glass is applied to thin-film solar cells industry, is commonly used for transparency electrode and the substrate of battery.The cost of transparent conducting glass accounts for 30% left and right of hull cell cost, so how to produce functional cheap transparent conducting glass, has become one of key of thin-film solar cells production.
For strengthening the photoabsorption of photovoltaic film battery, the nesa coating of conductive glass need to have the suede degree of nanoscale, and irregularity degree, makes light that diffuse scattering (conventionally measuring by haze value) occur when incident, increases light at the light path of inside battery transmission.A kind of novel U-shaped matte conductive glass need to be adsorbed in normal transparent conducting film surface as mask using nanometer ball by the method for immersion plating, by magnetron sputtering, in nanometer ball gap, increase again electrically conducting transparent film thickness, finally remove nanometer ball to obtain nano level U-shaped matte conductive glass (as shown in Figure 1).
Selecting of nanometer ball is one of technological core of U-shaped matte conductive glass, and on domestic and international market, can meet microspherulite diameter homogeneous, the manufacturer that controlled and film forming is even, density is high is very few.The height of the price of dispersed nano ball also makes the production cost of U-shaped matte conductive glass be difficult to reduce.
At present, relatively many methods for the preparation of polystyrene nano/micron ball have: dispersion copolymerization method, emulsion polymerization, seed swelling polymerization method etc.Seed swelling polymerization method, because its complex steps, condition are harsh and consuming time tediously long, is unfavorable for suitability for industrialized production; The polystyrene nanospheres particle diameter general requirement that is applied to novel matte conductive glass is at nano level (a small amount of micron order), and that this product cut size making with emulsion polymerization is sent out in dispersion polymerization is excessive.Therefore, only have on the market the polystyrene nanospheres that can meet the demands of minute quantity, and its higher price has directly caused the production cost of novel matte conductive glass greatly to increase.
Summary of the invention
In order to meet the processing requirement of Novel U-shaped matte conductive glass, for market provides how selectable, functional, cheap polystyrene nanospheres, the invention provides a kind of preparation method for being applied to the polystyrene nanospheres of novel matte conductive glass simultaneously.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is to provide a kind of preparation method who is applied to the polystyrene nanospheres of novel matte conductive glass, step 1): raw-material purifying, vinylbenzene is removed to stopper with the aqueous sodium hydroxide solution of 5wt%, with ultrapure water, be washed till neutrality afterwards, through anhydrous magnesium sulfate, dewater again, finally carrying out underpressure distillation, to be placed on refrigerator standby, and initiator obtains the initiator after purifying by ultrapure water secondary recrystallization by room temperature vacuum-drying; Step 2): polystyrene nanospheres synthetic, the vinylbenzene of treated mistake and ultrapure water are mixed in four-hole boiling flask, under nitrogen protection, being heated to 70-80 ℃ stirs 30 minutes, add afterwards initiator solution and react 5-12 hour, wherein, the concentration of vinylbenzene and initiator respectively: vinylbenzene 0.5-0.9mM, initiator 1.8-2.8mM; Step 3): after reaction finishes, nanometer ball stoste is cooled to room temperature, by ultracentrifugal method, obtain throw out, again after a series of processing, it is 5-15% that throw out is added to solvent cut to the massfraction of nanometer ball, obtaining particle diameter is 300-600nm, meets the polystyrene nanospheres suspension of application-specific.
In the preparation method of above-mentioned a kind of polystyrene nanospheres that is applied to novel matte conductive glass, initiator described in step 1) is Potassium Persulphate or ammonium persulphate.
In the preparation method of above-mentioned a kind of polystyrene nanospheres that is applied to novel matte conductive glass, step 2) after water mixes with vinylbenzene, can carry out ultrasonic emulsification process.
In the preparation method of above-mentioned a kind of polystyrene nanospheres that is applied to novel matte conductive glass, step 2) in, can add in addition vinylformic acid and vinylbenzene to carry out copolymerization, its content is 10-15mM.
In the preparation method of above-mentioned a kind of polystyrene nanospheres that is applied to novel matte conductive glass, step 2) in, can add sodium-chlor aggregation process, to obtain larger particle diameter, its content is 3-16mM.
In the preparation method of above-mentioned a kind of polystyrene nanospheres that is applied to novel matte conductive glass, in step 3), can increase ultrasonic disruption disperses and filter operation, to reduce microballoon agglomeration in solution, to be conducive to realize solution list dispersion effect, thereby further improve the homogeneity that nanometer ball adsorbs on conducting film.
The polystyrene nanospheres regular shape that method provided by the invention is produced is full, particle diameter uniformity, and aftertreatment is simple, can more ideally meet the application requiring of novel matte conductive glass.
Accompanying drawing explanation
Fig. 1 is that polystyrene nanospheres acts on schematic diagram in novel matte conductive glass;
Fig. 2 is polystyrene nanospheres preparation feedback principle schematic;
Fig. 3 is the SEM photo of embodiment 1 gained polystyrene nanospheres;
Fig. 4 is the SEM photo of embodiment 2 gained polystyrene nanospheres;
Fig. 5 is the SEM photo of embodiment 3 gained polystyrene nanospheres;
Fig. 6 is the SEM photo of embodiment 4 gained polystyrene nanospheres;
Fig. 7 is for being applied to the pipe/polyhenylethylene nano nanometer ball making in novel matte conductive glass AFM figure;
Fig. 8 is for being applied to the pipe/polyhenylethylene nano nanometer ball making in novel matte conductive glass AFM figure.
Embodiment
The present invention adopts emulsifier-free emulsion polymerization method, and for the application of novel matte conductive glass, synthesis technique has been done to some and adjusted targetedly.It has not only overcome other conventional synthesis method complicated operation, consuming time tediously long, the problems such as apparatus expensive and with an organic solvent contaminate environment health risk, the polystyrene nanospheres regular shape of simultaneously producing by the method is full, particle diameter uniformity, aftertreatment is simple, can more ideally meet the application requiring of novel matte conductive glass.
The invention discloses a kind of preparation method who is applied to the polystyrene nanospheres of novel matte conductive glass.The present invention be take vinylbenzene as monomer, adopts emulsifier-free emulsion polymerization method, prepares polystyrene nanospheres.Comprise the following steps: step 1): raw-material purifying, vinylbenzene is removed to stopper with the aqueous sodium hydroxide solution of 5wt%, with ultrapure water, be washed till neutrality afterwards, through anhydrous magnesium sulfate, dewater again, finally carrying out underpressure distillation, to be placed on refrigerator standby, and initiator obtains the initiator after purifying by ultrapure water secondary recrystallization by room temperature vacuum-drying; Step 2): polystyrene nanospheres synthetic, the vinylbenzene of treated mistake and ultrapure water are mixed in four-hole boiling flask, under nitrogen protection, being heated to 70-80 ℃ stirs 30 minutes, add afterwards initiator solution and react 5-12 hour, wherein, the concentration of vinylbenzene and initiator respectively: vinylbenzene 0.5-0.9mM, initiator 1.8-2.8mM; Step 3): after reaction finishes, nanometer ball stoste is cooled to room temperature, by ultracentrifugal method, obtain throw out, again after a series of processing, it is 5-15% that throw out is added to solvent cut to the massfraction of nanometer ball, obtaining particle diameter is 300-600nm, meets the polystyrene nanospheres suspension of application-specific.
In step 1), initiator is Potassium Persulphate or ammonium persulphate.
In step 2) after water mixes with vinylbenzene, can carry out ultrasonic emulsification process.
In step 2) in can add in addition vinylformic acid and vinylbenzene to carry out copolymerization, its content is 10-15mM.
In step 2) in can add sodium-chlor aggregation process, to obtain larger particle diameter, its content is 3-16mM.
In step 3), can increase ultrasonic disruption and disperse and filter operation, to reduce microballoon agglomeration in solution, to be conducive to realize solution list dispersion effect, thereby further improve the homogeneity that nanometer ball adsorbs on conducting film.
Below in conjunction with accompanying drawing and embodiment, with regard to the present invention, do further detailed description:
Embodiment 1:
1400mL water and 156mL vinylbenzene are added in four-hole boiling flask successively; Mix and blend and pass into nitrogen, simultaneously heating in water bath is warming up to 80 ℃; After constant temperature 30min, add potassium persulfate solution (0.95g Potassium Persulphate/44mL water), at 80 ℃, react 12 hours; Reacted cooling after, whizzer to reaction stoste centrifugal 20min, removes supernatant liquid afterwards and repeats centrifugally operated 4 times under the condition of 8000rpm; With ultrasonic disruption instrument by the ultrasonic dispersion treatment 20min of microspheres solution; Nanometer ball suspension after supersound process is diluted to needed concentration.Fig. 3 is the SEM photo of embodiment 1 obtained polystyrene nanospheres.
Embodiment 2:
1400mL water, a small amount of acrylic acid solution and 179mL vinylbenzene are added in four-hole boiling flask successively; Mix and blend and pass into nitrogen, simultaneously heating in water bath is warming up to 80 ℃; After constant temperature 30min, add potassium persulfate solution (0.95g Potassium Persulphate/44mL water), at 80 ℃, react 7 hours; Reacted cooling after, whizzer to reaction stoste centrifugal 20min, removes supernatant liquid afterwards and repeats centrifugally operated 4 times under the condition of 8000rpm; With ultrasonic disruption instrument by the ultrasonic dispersion treatment 20min of microspheres solution; Nanometer ball suspension after supersound process is diluted to needed concentration.Fig. 4 is the SEM photo of embodiment 2 obtained polystyrene nanospheres.
Embodiment 3:
1400mL water, sodium chloride aqueous solution (0.7g sodium-chlor/10ml water) and 100mL vinylbenzene are added in four-hole boiling flask successively; Mix and blend and pass into nitrogen, simultaneously heating in water bath is warming up to 75 ℃; After constant temperature 30min, add potassium persulfate solution (0.95g Potassium Persulphate/44mL water), at 80 ℃, react 7 hours; Reacted cooling after, whizzer to reaction stoste centrifugal 20min, removes supernatant liquid afterwards and repeats centrifugally operated 4 times under the condition of 8000rpm; With ultrasonic disruption instrument by the ultrasonic dispersion treatment 20min of microspheres solution; Nanometer ball suspension after supersound process is diluted to needed concentration.Fig. 5 is the SEM photo of embodiment 3 obtained polystyrene nanospheres.
Embodiment 4:
1400mL water, sodium chloride aqueous solution (0.7g sodium-chlor/10ml water) and 156mL vinylbenzene are added in four-hole boiling flask successively; Mix and blend and pass into nitrogen, simultaneously heating in water bath is warming up to 75 ℃; After constant temperature 30min, add potassium persulfate solution (0.95g Potassium Persulphate/44mL water), at 75 ℃, react 7 hours; Reacted cooling after, whizzer to reaction stoste centrifugal 20min, removes supernatant liquid afterwards and repeats centrifugally operated 4 times under the condition of 8000rpm; With ultrasonic disruption instrument by the ultrasonic dispersion treatment 20min of microspheres solution; Nanometer ball suspension after supersound process is diluted to needed concentration.Fig. 6 is the SEM photo of embodiment 4 obtained polystyrene nanospheres.
The present invention is not limited to above-mentioned preferred forms, and anyone should learn the structural changes of making under enlightenment of the present invention, and every have identical or close technical scheme with the present invention, within all falling into protection scope of the present invention.
Claims (6)
1. be applied to a preparation method for the polystyrene nanospheres of novel matte conductive glass, it is characterized in that comprising the following steps:
Step 1): raw-material purifying, vinylbenzene is removed to stopper with the aqueous sodium hydroxide solution of 5wt%, with ultrapure water, be washed till neutrality afterwards, through anhydrous magnesium sulfate, dewater again, finally carrying out underpressure distillation, to be placed on refrigerator standby, and initiator obtains the initiator after purifying by ultrapure water secondary recrystallization by room temperature vacuum-drying;
Step 2): polystyrene nanospheres synthetic, the vinylbenzene of treated mistake and ultrapure water are mixed in four-hole boiling flask, under nitrogen protection, being heated to 70-80 ℃ stirs 30 minutes, add afterwards initiator solution and react 5-12 hour, wherein, the concentration of vinylbenzene and initiator respectively: vinylbenzene 0.5-0.9mM, initiator 1.8-2.8mM;
Step 3): after reaction finishes, nanometer ball stoste is cooled to room temperature, by ultracentrifugal method, obtain throw out, again after a series of processing, it is 5-15% that throw out is added to solvent cut to the massfraction of nanometer ball, obtaining particle diameter is 300-600nm, meets the polystyrene nanospheres suspension of application-specific.
2. according to the preparation method of the polystyrene nanospheres that is applied to novel matte conductive glass described in right 1, it is characterized in that: initiator described in step 1) is Potassium Persulphate or ammonium persulphate.
3. according to the preparation method of the polystyrene nanospheres that is applied to novel matte conductive glass described in right 1, it is characterized in that: step 2) after water mixes with vinylbenzene, can carry out ultrasonic emulsification process.
4. according to the preparation method of the polystyrene nanospheres that is applied to novel matte conductive glass described in right 1, it is characterized in that: step 2) in can add in addition vinylformic acid and vinylbenzene to carry out copolymerization, its content is 10-15mM.
5. according to the preparation method of the polystyrene nanospheres that is applied to novel matte conductive glass described in right 1, it is characterized in that: step 2) in can add sodium-chlor aggregation process, to obtain larger particle diameter, its content is 3-16mM.
6. according to the preparation method of the polystyrene nanospheres that is applied to novel matte conductive glass described in right 1, it is characterized in that: in step 3), can increase ultrasonic disruption and disperse and filter operation, to reduce microballoon agglomeration in solution, to be conducive to realize solution list dispersion effect, thereby further improve the homogeneity that nanometer ball adsorbs on conducting film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106653914A (en) * | 2016-12-22 | 2017-05-10 | 浙江大学 | Ultra-thin sunlight heater and preparation method therefor |
| CN107082837A (en) * | 2017-05-12 | 2017-08-22 | 山东大学 | A kind of preparation method of particle diameter and the controllable monodisperse polystyrene microsphere of surface charge |
Citations (3)
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| CN101582469A (en) * | 2009-03-24 | 2009-11-18 | 新奥光伏能源有限公司 | Method for attaching matte transparent conductive film on substrate |
| US20110111598A1 (en) * | 2009-11-09 | 2011-05-12 | Chia-Hua Chan | Method for preparing patterned substrate by using nano- or micro- particles |
| CN102254961A (en) * | 2011-05-28 | 2011-11-23 | 惠州市易晖太阳能科技有限公司 | Conductive suede glass special for solar cells, and preparation method and application thereof |
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2013
- 2013-10-15 CN CN201310481710.6A patent/CN103570849A/en active Pending
Patent Citations (3)
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| CN101582469A (en) * | 2009-03-24 | 2009-11-18 | 新奥光伏能源有限公司 | Method for attaching matte transparent conductive film on substrate |
| US20110111598A1 (en) * | 2009-11-09 | 2011-05-12 | Chia-Hua Chan | Method for preparing patterned substrate by using nano- or micro- particles |
| CN102254961A (en) * | 2011-05-28 | 2011-11-23 | 惠州市易晖太阳能科技有限公司 | Conductive suede glass special for solar cells, and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106653914A (en) * | 2016-12-22 | 2017-05-10 | 浙江大学 | Ultra-thin sunlight heater and preparation method therefor |
| CN107082837A (en) * | 2017-05-12 | 2017-08-22 | 山东大学 | A kind of preparation method of particle diameter and the controllable monodisperse polystyrene microsphere of surface charge |
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