CN100434486C - Method for preparing hypovanadic oxide suspensoid - Google Patents
Method for preparing hypovanadic oxide suspensoid Download PDFInfo
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- CN100434486C CN100434486C CNB2006101170274A CN200610117027A CN100434486C CN 100434486 C CN100434486 C CN 100434486C CN B2006101170274 A CNB2006101170274 A CN B2006101170274A CN 200610117027 A CN200610117027 A CN 200610117027A CN 100434486 C CN100434486 C CN 100434486C
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- suspensoid
- powder
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- hypovanadic oxide
- wetting
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Abstract
The invention relates to VO2 powdery stable suspension with average particle diameter 70nm used (NaPO3)6 as dispersant. Anionic polyelectrolyte makes the VO2 powdery isoelectric point reduce. Ultrasonic dispersion improves the dispersant distribution on particle surface to obviously change the suspension rheological property. It is proved by detecting suspension Zeta electrical potential that the (NaPO3)6 can greatly increase particle surface electric quantity. While pH is 10, the VO2 powdery suspension is stable; the optimum use level of the (NaPO3)6 dispersant is 0.8wt%.
Description
Technical field
The invention belongs to paint field, relate more specifically to powder coating.
Background technology
Nano-powder typically refers to grain graininess at 1～100nm, small solid particulate between microcosmic particle and macro object.Nano-powder is because of its volume effect is led at magnetic, catalytic, photoabsorption, electricity with surface effects, hardness is compared with conventional material with aspects such as fusing points and demonstrated exceptional function, thereby receives people's very big concern.But, because little, specific surface area of particle diameter of nanometer powder and total surface can be all very big, reunite easily in solution, the existence of reunion will hinder giving full play to of nano-powder advantage again greatly, and dispersion, the stability of therefore studying nano-powder will be the prerequisite and the bases of further improving material property.According to the dispersion medium difference, dispersion system can be divided into water-based system (water is medium) and non-aqueous system (is matter with the organic solvent).Nanometer VO
2The particle specific surface area is very big, and the coordination wretched insufficiency.Thereby show extremely strong surfactivity, reunite very easily mutually.Form big aggregate, thereby influence practical application effect.It is to add organic surface active agent etc. in aqueous solution that nano powder surface is handled method commonly used, makes it coat, be adsorbed on nano grain surface effectively.That the dispersion of nano-powder in aqueous solvent comprises is wetting, dispersion and stably dispersing three phases.Because gravitational effect makes VO between Van der Waals force and particle
2Powder particle closely concentrates at and forms soft aggregate together, and when this aggregate immersed liquid medium, refusal disperseed so that the form of poly-group is wetted.Therefore, have only as nanometer VO
2By abundant when wetting, it could be spread out well between the particle.And anion surfactant is adsorbed on the capillary wall with hydrophobic group on a solid liquid interface, hydrophilic group stretches in the liquid, the interfacial tension at a solid liquid interface is reduced significantly, and improved the consistency at a solid liquid interface, cause slit place wetting ability to strengthen, it is wetting around independently primary partical or less aggregate to help aqueous medium.Along with the increase of place, particle agglomeration crack seepage water pressure, in conjunction with the extraneous mechanical shear stress that is provided, can open nanometer VO again
2Aggregate.Make powder obtain better to disperse.Anion surfactant his-and-hers watches bread has covered the nanometer VO of sieve and silica-sesquioxide in water-based system
2Wetting preferably dissemination is arranged.But, be not that any surface treatment agent can both promote liquid infiltration, dissimilar surface treatment agents role in the dispersion process of particle agglomeration is different.
VO
2It is a kind of phase-change metal oxide compound, reduction along with temperature, greatly about 68 ℃, flipflop from metal to nonmetal (or semi-conductor) character takes place in material, the sudden change of 4～5 orders of magnitude takes place in resistivity, also be accompanied by the sudden change of tangible optical transmittance simultaneously, the transformation (as figure below) from the four directions to the monocline takes place in its crystalline structure.These phase-change characteristics make VO
2Can be applied to buildings sun power temperature control unit, photoelectric switch material, thermistor material, can wipe fields such as optical memory material, blinding laser weapons safety guard, photochromic material, submillimeter wave radiating modulator, polarizer and variable mirror.
Because VO
2Cause the change of IR transmittance before and after the powder phase transformation, we can be with VO
2Powder is coated on forms such as buildings, automobile surface and comes temperature in the automatic surge chambers, thus save energy effectively.When temperature when transformation temperature is following, the infrared light transmitance is higher, and room temp is raise; When temperature rises to transformation temperature when above, VO
2Undergo phase transition, the transmitance of infrared light is reduced, reflectivity improves, and room temp reduces gradually.Circulation just can be played temperature automatically controlled effect and so forth.Common VO
2Transformation temperature is higher than room temperature, but by mixing transformation temperature is reduced near the room temperature, just in time satisfies application requiring.
Utilize VO
2The mutagenicity of resistance before and after the phase transformation, VO
2Can be used as that heat is touched switch or heat is touched transmitter.When temperature is lower than transformation temperature, VO
2Be in high-resistance semi-conductor state, circuit is disconnected; When temperature is higher than transformation temperature, VO
2Be low-resistance metallic state, circuit is connected.This just realizes automatic control to circuit by material by temperature-induced variations.General surface film material can adapt to the job requirement of low current, and adopts VO
2The stupalith that powder is made can bear the Working environment of big electric current, and use range is wider.
But if can make nanometer VO
2In coating, obtain better application, at first will solve nanometer VO
2The problem of the dispersing uniformity in the aqueous systems solvent, existing nanometer VO
2Adopt sodium dodecyl benzenylsulfonate mostly, the short practical application effect that can not get of its time.
Summary of the invention
The technical problem that will solve required for the present invention just provides a kind of nanometer VO that allows
2Evenly be suspended in the method in the aqueous systems solvent, so that nanometer VO
2The powder better application is in water-borne coatings.
The technical scheme that solves the technology of the present invention problem is as follows:
A kind of preparation method of hypovanadic oxide suspensoid, this method comprises the steps:
A, with a small amount of wetting agent with VO
2Powder is wetting;
B, with an amount of (NaPO of water dissolution
3)
6
The C, (NaPO after will dissolving
3)
6Add wetting VO
2In, (NaPO wherein
3)
6Account for 0.1%～2% of total solution weight, the two is sheared mixed, regulate pH value to 7～11 in the mixing process; D, the solution of C step gained is vibrated, and stir, promptly get uniform hypovanadic oxide suspensoid.
Wherein wetting nanometer VO
2The used wetting agent of powder is with just drenched for best, and used wetting agent can be a hydrophobic long carbochain ethoxy compound etc.
Be to shear mixedly with the rotating speed of 5000r/min in the C step, in whipping process, add the pH value of ammoniacal liquor regulator solution
The pH value of solution preferably is adjusted to 10 in the described C step, prepared VO
2Powder suspension is the most stable.
Described D step adopts ultra-sonic oscillation, and duration of oscillation is 15-30 minute.
The present invention is with (NaPO
3)
6For dispersion agent has prepared median size is the VO of 70nm
2The stable suspension of powder, anionic polyelectrolyte makes VO
2The powder iso-electric point has reduced; The ultrasonic dispersing improved effect distribution of dispersion agent at particle surface, Gu and make the rheological of suspension that tangible change be arranged.(NaPO
3)
6Significantly improve the particle surface carried charge, when pH 10 the time, VO
2The powder effect suspension stabilization.Rheometer test has been determined the preparation stable suspension when pH=10, required the best (NaPO
3)
6Dispersant dosage is 0.8wt%, VO
2The powder effect suspension stabilization.The invention has the advantages that cost is low simple to operate, be suitable for water-based system.
Description of drawings
Fig. 1 is nanometer VO of the present invention
2Its zeta-potential of powder suspension different ratios is with pH value variation diagram;
Fig. 2 is nanometer VO of the present invention
2Powder suspension under various different PH its zeta-potential with (NaPO
3)
6Variation diagram.
Embodiment
How further specify the present invention below in conjunction with specific embodiment realizes:
Embodiment 1
Take by weighing 1g nanometer VO
2Powder, it is wetting to add 5 wetting agents, takes by weighing 0.8g (NaPO again
3)
6Be mixed with solution with the 100g water dissolution, solution added wetting good nanometer VO is housed
2In the powder beaker, mix with the 5000r/min shearing, and regulate its pH value to 10, stir 2h, use ultra-sonic oscillation 30min, promptly get nanometer VO with ammoniacal liquor
2The powder unit for uniform suspension.Its zeta-potential is seen Fig. 1 and Fig. 2.
Embodiment 2
Take by weighing 2g nanometer VO2 powder, it is wetting to add 10 wetting agents, take by weighing 1.6g (NaPO3) 6 usefulness 200g water dissolution again and be mixed with solution, the solution adding is equipped with in the wetting good nanometer VO2 powder beaker, mix with the 5000r/min shearing, and regulate its pH value to 9, stir 2h with ammoniacal liquor, use ultra-sonic oscillation 30min, promptly get nanometer VO2 powder unit for uniform suspension.
Claims (7)
1, a kind of preparation method of hypovanadic oxide suspensoid, this method comprises the steps:
A, with a small amount of wetting agent with VO
2Powder is wetting;
B, with an amount of (NaPO of water dissolution
3)
6
The C, (NaPO after will dissolving
3)
6Add wetting VO
2In, (NaPO wherein
3)
6Account for 0.1%～2% of total solution weight, the two is sheared mixed, regulate pH value to 7～11 in the mixing process;
D, the solution of C step gained is vibrated, and stir, promptly get the VO that median size is 70nm
2The stable suspension of powder.
2, the preparation method of a kind of hypovanadic oxide suspensoid as claimed in claim 1 is characterized in that: wetting nanometer VO
2The used wetting agent of powder is as the criterion just to drench, and used wetting agent can be hydrophobic long carbochain ethoxy compound.
3, the preparation method of a kind of hypovanadic oxide suspensoid as claimed in claim 1 is characterized in that: shear mixed with the rotating speed of 5000r/min in the C step.
4, the preparation method of a kind of hypovanadic oxide suspensoid as claimed in claim 1 is characterized in that, uses the pH value of ammoniacal liquor regulator solution in the C step.
5, the preparation method of a kind of hypovanadic oxide suspensoid as claimed in claim 1 is characterized in that: reconcile pH value to 10 in the described C step.
6, the preparation method of a kind of hypovanadic oxide suspensoid as claimed in claim 1 is characterized in that: described D step adopts ultra-sonic oscillation.
7, the preparation method of a kind of hypovanadic oxide suspensoid as claimed in claim 6 is characterized in that: duration of oscillation 15-30 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101170274A CN100434486C (en) | 2006-10-11 | 2006-10-11 | Method for preparing hypovanadic oxide suspensoid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101170274A CN100434486C (en) | 2006-10-11 | 2006-10-11 | Method for preparing hypovanadic oxide suspensoid |
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| Publication Number | Publication Date |
|---|---|
| CN1935909A CN1935909A (en) | 2007-03-28 |
| CN100434486C true CN100434486C (en) | 2008-11-19 |
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ID=37953657
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101170274A Expired - Fee Related CN100434486C (en) | 2006-10-11 | 2006-10-11 | Method for preparing hypovanadic oxide suspensoid |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073941B (en) * | 2012-01-19 | 2014-09-10 | 中国科学院上海硅酸盐研究所 | Vanadium dioxide powder slurry and preparation method thereof |
| CN103073942B (en) * | 2012-01-19 | 2014-09-10 | 中国科学院上海硅酸盐研究所 | Vanadium dioxide composite powder and preparation method thereof |
| CN103073943B (en) | 2012-01-19 | 2014-09-17 | 中国科学院上海硅酸盐研究所 | Vanadium dioxide intelligent temperature control coating |
| CN103191589B (en) * | 2013-02-20 | 2014-12-10 | 东南大学 | Preparation method for nano-fluid based on specific absorbance |
| CN109923144B (en) * | 2016-11-07 | 2022-03-22 | 湛新荷兰有限公司 | Process for preparing thixotropic compositions |
| CN107597017B (en) * | 2017-09-28 | 2019-12-10 | 江南大学 | Preparation method of nano vanadium dioxide compound dispersant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1279211A (en) * | 2000-08-04 | 2001-01-10 | 中山大学 | Process for preparing nm-class VO2 powder and nm-class ceramics |
| CN1621459A (en) * | 2004-10-28 | 2005-06-01 | 中山大学 | Intelligent vanadium dioxide solar temperature control coating |
-
2006
- 2006-10-11 CN CNB2006101170274A patent/CN100434486C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1279211A (en) * | 2000-08-04 | 2001-01-10 | 中山大学 | Process for preparing nm-class VO2 powder and nm-class ceramics |
| CN1621459A (en) * | 2004-10-28 | 2005-06-01 | 中山大学 | Intelligent vanadium dioxide solar temperature control coating |
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| CN1935909A (en) | 2007-03-28 |
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Granted publication date: 20081119 Termination date: 20121011 |