CN102604122B - Preparation method of pomegranate-shaped composite nano particles - Google Patents
Preparation method of pomegranate-shaped composite nano particles Download PDFInfo
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- CN102604122B CN102604122B CN 201210091714 CN201210091714A CN102604122B CN 102604122 B CN102604122 B CN 102604122B CN 201210091714 CN201210091714 CN 201210091714 CN 201210091714 A CN201210091714 A CN 201210091714A CN 102604122 B CN102604122 B CN 102604122B
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- silicon dioxide
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Abstract
The invention relates to a preparation method of pomegranate-shaped composite nano particles. The invention aims to provide the preparation method of the pomegranate-shaped composite nano particles. In the composite nano particles (PVA (Polyvinyl Alcohol) @SiO2), PVA is used as a core; SiO2 nano particles are self-assembled on the spherical surface of the PVA to form pomegranate-shaped structures which are regularly arranged; and the prepared composite nano particles have smooth appearance, uniform size distribution and controllable particle sizes. The invention adopts the technical scheme that the preparation method of the pomegranate-shaped composite nano particles is characterized by comprising the following steps of: (1) preparing aqueous solution of the PVA; (2) preparing SiO2 nano particle ethanol dispersion solution; and (3) preparing the composite nano particles in a high voltage electric field. The preparation method is suitable for rubber modification, engineering plastics, ceramics, biomedicine, optics, building material coatings, modification of resin-based composite materials and the like.
Description
Technical field
The present invention relates to a kind of employing Nano particles of silicon dioxide and (use SiO
2Expression) composite nanoparticle of coating polyvinyl alcohol (representing with PVA) acquisition pomegranate shape (is used PVASiO
2Expression) preparation method.Be applicable to modified rubber, engineering plastics, pottery, biomedicine, optics, building materials coating, polymer matrix composites modification etc.
Background technology
Because nano material has small-size effect, surface-interface effect, quantum size effect and macroscopic quantum channel effect and special optical and electrical properties.The research of nano material more and more is subject to people's favor, and nano silicon is to use one of nano material early, about nanometer SiO
2Application in modified rubber, engineering plastics, pottery, biomedicine, optics, building materials coating, polymer matrix composites modification had many reports.For example, the small-size effect of nano silicon and macro quanta tunnel effect make it produce the effect of oozing of becoming silted up, can be deep near the unsaturated link(age) of macromolecular chain, and and the electronic cloud of unsaturated link(age) have an effect, improve heat, light stability and the chemical stability of macromolecular material, thereby improve resistance to deterioration and the chemical resistant properties of product.But nano silicon widespread use every field has broad application prospects and huge commercial value.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of preparation method of composite nanoparticle of pomegranate shape, this composite nanoparticle (PVASiO
2) take polyvinyl alcohol (PVA) as nuclear, Nano particles of silicon dioxide (SiO
2) in the pomegranate shape structure of polyvinyl alcohol ball surface self-organization formation arrangement regulation, the composite nanoparticle profile that makes is round and smooth, size distribution is even, particle diameter is controlled.
The technical solution adopted in the present invention is: the preparation method of the composite nanoparticle of pomegranate shape is characterized in that comprising step:
(1) preparation of polyvinyl alcohol water solution:
Selecting molecular weight is the polyvinyl alcohol of 6-12 ten thousand, adding the concentration that water is mixed with polyvinyl alcohol is the polyvinyl alcohol water solution of 4%-15% (weight), then after polyvinyl alcohol water solution being stirred 18～24 hours at normal temperatures, again 90 ℃-120 ℃ stirring heating 3-5 hour, be cooled to after the room temperature for subsequent use;
(2) preparation of Nano particles of silicon dioxide alcohol dispersion liquid:
Nano particles of silicon dioxide is mixed with ethanol, and the concentration that is mixed with Nano particles of silicon dioxide is the Nano particles of silicon dioxide alcohol dispersion liquid of 5%～15% (weight), and ultra-sonic dispersion 1-5 hour for subsequent use;
(3) preparation process of composite nanoparticle under the high-voltage electric field:
Described polyvinyl alcohol water solution and Nano particles of silicon dioxide alcohol dispersion liquid are placed respectively the inside and outside layer of metal coaxial injectors syringe needle, internal layer is polyvinyl alcohol water solution, and skin is the Nano particles of silicon dioxide alcohol dispersion liquid;
One of high-voltage electric field is terminated on the coaxial injectors, make its positively charged, the other end ground connection of high-voltage electric field consists of high-voltage electric field, and the above-mentioned internal layer that this moment is charged and the mixing solutions in the skin spray to ground terminal under the driving of electric field;
Internal layer solution fltting speed is 0.6-1.4ml/h in the preparation process, and outer solution fltting speed is 1.2-4ml/h, and accepting distance is 10-20cm, and voltage is 18-35kv, and electric current is 1-2mA.
The invention has the beneficial effects as follows:
(1) the inventive method is utilized the PVA water soluble, but is insoluble to the characteristics of the organic solvents such as ethanol, prepares respectively the PVA aqueous solution and SiO
2Alcohol dispersion liquid, and under the high-voltage electric field effect, prepare the PVASiO that diameter is 30nm-200nm
2, wherein take PVA as nuclear, SiO
2Form special pomegranate shape structure, the PVASiO that makes at PVA ball surface self-organization
2Size distribution is even, profile is round and smooth, particle diameter is controlled and the SiO on PVA surface
2Arrangement regulation.
(2) present method preparation process is simple, can be used in a large number fast PVASiO
2Preparation, and preparation cycle is short.
(3) method of employing high voltage field can be SiO
2Cover on the receiving device of any shape, coating is even.
Description of drawings
Fig. 1 is the apparatus structure schematic diagram that the present invention adopts when preparing.
The pomegranate shape PVASiO that Fig. 2-the 3rd, the present invention make
2Scanning electron microscope (SEM) photograph (Fig. 3 is magnifying state).
Embodiment
The present embodiment prepares the composite nanoparticle (PVASiO of pomegranate shape
2) may further comprise the steps:
1, preparation polyvinyl alcohol (PVA) aqueous solution: the PVA (wherein the PVA molecular weight is 80000) of 0.86g is dissolved in the water, being mixed with PVA concentration is the PVA aqueous solution of 10% (weight percent), then after the PVA aqueous solution being stirred 20 hours at normal temperatures, again 100 ℃ of left and right sides stirring heating 4 hours, be cooled to after the room temperature for subsequent use;
2, preparation Nano particles of silicon dioxide (SiO
2) alcohol dispersion liquid: with the SiO of 0.96g
2Be dispersed in the ethanol, be mixed with SiO
2Concentration be the SiO of 10% (weight percent)
2Alcohol dispersion liquid, ultra-sonic dispersion 3 hours is for subsequent use;
3, as shown in Figure 1, the PVA aqueous solution is injected the internal layer (thruster 2) of metal coaxial injectors, with SiO
2Alcohol dispersion liquid is injected the skin (thruster 1) of metal coaxial injectors; Again one of high-voltage electric field is terminated on the metal coaxial injectors, make its positively charged, the other end ground connection of high-voltage electric field, consist of high-voltage electric field, this routine voltage is 25kv, and the fltting speed of internal layer syringe is 0.5ml/h, the fltting speed of outer syringe is 4ml/h, spray to ground terminal after two kinds of solution parcels of exit end of syringe mix, accepting distance is 10-20cm, can make the PVASiO of pomegranate shape at ground terminal
2
Because the internal layer PVA aqueous solution is insoluble to outer SiO
2Alcohol dispersion liquid, therefore internal layer PVA aqueous solution balling-up under surface tension effects, and by outer SiO
2The alcohol dispersion liquid parcel.Such composite particles is when spraying to ground terminal, and aqueous solvent and ethanol evaporate together, last SiO
2The hydroxyl on surface and the hydroxyl on PVA surface form hydrogen bond and self-assemble to PVA bead surface, thereby make the composite particles of the Nano particles of silicon dioxide coating polyvinyl alcohol of pomegranate shape.
Fig. 2, Fig. 3 are the pomegranate shape PVASiO of preparation
2Scanning electron microscope (SEM) photograph, wherein Fig. 3 is the enlarged view of pomegranate shape nanoparticle.
Claims (1)
1. the preparation method of the composite nanoparticle of a pomegranate shape is characterized in that comprising step:
(1) preparation of polyvinyl alcohol water solution:
Selecting molecular weight is the polyvinyl alcohol of 6-12 ten thousand, adding the concentration that water is mixed with polyvinyl alcohol is the polyvinyl alcohol water solution of 4 ~ 15% weight, then after polyvinyl alcohol water solution being stirred 18 ~ 24 hours at normal temperatures, again 90 ℃-120 ℃ stirring heating 3-5 hour, be cooled to after the room temperature for subsequent use;
(2) preparation of Nano particles of silicon dioxide alcohol dispersion liquid:
Nano particles of silicon dioxide is mixed with ethanol, and the concentration that is mixed with Nano particles of silicon dioxide is the Nano particles of silicon dioxide alcohol dispersion liquid of 5 ~ 15% weight, and ultra-sonic dispersion 1-5 hour for subsequent use;
(3) preparation process of composite nanoparticle under the high-voltage electric field:
Described polyvinyl alcohol water solution and Nano particles of silicon dioxide alcohol dispersion liquid are placed respectively the ectonexine of metal coaxial injectors syringe needle, internal layer is polyvinyl alcohol water solution, and skin is the Nano particles of silicon dioxide alcohol dispersion liquid;
One of high-voltage electric field is terminated on the coaxial injectors, make its positively charged, the other end ground connection of high-voltage electric field consists of high-voltage electric field, and the above-mentioned internal layer that this moment is charged and the mixing solutions in the skin spray to ground terminal under the driving of electric field;
Internal layer solution fltting speed is 0.6-1.4mL/h in the preparation process, and outer solution fltting speed is 1.2-4mL/h, and accepting distance is 10-20cm, and voltage is 18-35kv, and electric current is 1-2mA.
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| CN 201210091714 CN102604122B (en) | 2012-03-30 | 2012-03-30 | Preparation method of pomegranate-shaped composite nano particles |
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| CN103012808A (en) * | 2012-12-21 | 2013-04-03 | 浙江理工大学 | Preparation method of super-hydrophobic particles |
| JP6674801B2 (en) * | 2016-03-09 | 2020-04-01 | 信濃電気製錬株式会社 | Composite particles for abrasive grains and method for producing abrasives and composite particles for abrasive grains using the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080210302A1 (en) * | 2006-12-08 | 2008-09-04 | Anand Gupta | Methods and apparatus for forming photovoltaic cells using electrospray |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20080210302A1 (en) * | 2006-12-08 | 2008-09-04 | Anand Gupta | Methods and apparatus for forming photovoltaic cells using electrospray |
Non-Patent Citations (4)
| Title |
|---|
| "从电纺丝到电喷离子化制备核壳纳米粒子";郝秀峰等;《高等学校化学学报》;20050228;第26卷(第2期);第385-387页 * |
| 洪友良等."二氧化硅@聚合物同轴纳米纤维".《高等学校化学学报》.2005,第26卷(第5期), |
| 洪友良等."二氧化硅聚合物同轴纳米纤维".《高等学校化学学报》.2005,第26卷(第5期), * |
| 郝秀峰等."从电纺丝到电喷离子化制备核壳纳米粒子".《高等学校化学学报》.2005,第26卷(第2期), |
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