CN107189583B - A kind of nanometer heat isolation paint - Google Patents
A kind of nanometer heat isolation paint Download PDFInfo
- Publication number
- CN107189583B CN107189583B CN201710487267.1A CN201710487267A CN107189583B CN 107189583 B CN107189583 B CN 107189583B CN 201710487267 A CN201710487267 A CN 201710487267A CN 107189583 B CN107189583 B CN 107189583B
- Authority
- CN
- China
- Prior art keywords
- antimony
- kernel
- powder
- nano powder
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2231—Oxides; Hydroxides of metals of tin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of nanometer heat isolation paints, it is characterised by comprising: water-borne acrylic coatings and making an addition to compound nuclear shell structure nano powder in the water-borne acrylic coatings, the compound nuclear shell structure nano powder includes: the first kernel, and first kernel is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 1%~10%；Middle layer, the middle layer are the silicon dioxide layer being coated on outside first kernel, and first kernel and middle layer constitute intermediate powder；Outer layer, the outer layer are the antimony doped stannic oxide nano powder layer that the antimony mole doping concentration being coated on outside the intermediate powder is 5%~15%.The production equipment and process method of the nanometer heat isolation paint is simple, and economic cost is low.The insulating moulding coating with compound nuclear shell structure nano powder that this method is prepared, the dispersibility of powder than using the insulating moulding coating of antimony doped stannic oxide nanometer material good merely, and heat insulation is also more preferably.
Description
Technical field
The present invention relates to a kind of insulating moulding coating, especially a kind of nanometer heat isolation paint.
Background technique
In recent years, hud typed hetero nano structure material is due to having different from any single substance property and materialized
It learns and field of nanometer technology has played extensive concern.Nucleocapsid hetero nano structure material can be by the material structure of different composition functions
At can construct more good composite functional material and device by Material cladding, complementation and optimization, meet the needs of development.
Core-shell structure material is formed in particle surface cladding shell substance, the interaction between control particle is can be very good, passes through
The composition for changing the size of coating, structure and particle can assign particle with special functional characteristic, so that it be made to obtain
More extensive potential application.
Stibium doping stannic oxide (Antimony tin oxide, abbreviation ATO) nano material, has combined ATO material
And the advantages of nano material, it has unique photoelectric properties, ionizing radiation-resistant, good antireflective, infrared absorption, thermostabilization
Property and very high ion selectivity exchange capacity is known as to certain members, can be used for insulating moulding coating, low-E glass for building,
Infrared absorption heat-barrier material, anti-static plastic, Radiation-proof antistatic coating material, fiber, electrode material, gas sensor etc..?
Foreign countries, especially in Japan, the U.S., the preparation and application study of ATO nano material come into the stage of large-scale production.
And the research of China in this respect is started late, product relies primarily on import.So the autonomous research of ATO nano material,
Become current considerable scientific research project.Huge economic benefit and social benefit, therefore, ATO have been involved among these
Its preparation and application of nano material are increasingly taken seriously.
ATO nano material is a kind of excellent transparent heat-insulated filler, has excellent light-coloured transparent and infrared absorption special
Property, and it is corrosion-resistant, thermal stability is high.However, it is desirable to heat-proof quality is further increased, in insulating moulding coating, researcher is by adding
A certain amount of inorganic nano-particle is added to be modified coating property.For example, the Chinese invention of Publication No. CN1563231A
Patent discloses a kind of be used as with nano ATO wet pulp and nano-indium stannum oxide (Indium Tin Oxide, abbreviation ITO) wet pulp and changes
Property filler be added in glass coating make coating have good visible light transmittance and very high infrared shielding effect.And
Nano-glass heat insulation paint need to only brush several microns of thickness, so that it may reach very good heat insulation, it is easy to operate
And it is cheap.ATO nanoparticle itself has good antireflective, the functions such as anti-radiation and infrared absorption, and its is good
Light transmittance, weatherability and stability and its cheap cost, so that the nanometer of its nanometer heat isolation paint for becoming present mainstream
Filler.It is saturating that the Chinese invention patent of Publication No. CN106118287A discloses a kind of nano ATO/CuS filler water soluble acrylic acid
It is bright heat-insulated, using nano ATO/CuS mixing filling, achieve the purpose that improving performance.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention proposes a kind of nanometer heat isolation paint.
For this purpose, a kind of nanometer heat isolation paint provided by the invention, comprising: water-borne acrylic coatings and make an addition to
Compound nuclear shell structure nano powder in the water-borne acrylic coatings, the compound nuclear shell structure nano powder includes: first
Kernel, first kernel are the antimony doped stannic oxide nano powder that antimony mole doping concentration is 1%~10%；Middle layer,
The middle layer is the silicon dioxide layer being coated on outside first kernel, and first kernel and middle layer constitute intermediate powder
Body；Outer layer, the outer layer are the Sb doped dioxy that the antimony mole doping concentration being coated on outside the intermediate powder is 5%~15%
Change tin nano-powder layer.
Preferably, first kernel is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 8.5%.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside second kernel is 5%
Tin oxide nano-powder layer.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside second kernel is 7%
Tin oxide nano-powder layer.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside second kernel is 10%
Tin oxide nano-powder layer.
Preferably, the outer layer is the Sb doped two that the antimony mole doping concentration being coated on outside second kernel is 15%
Tin oxide nano-powder layer.
Preferably, the mean grain size of the compound nuclear shell structure nano powder is between 1.726nm and 2.115nm.
Preferably, the mass parts ratio of the compound nuclear shell structure nano powder and water-borne acrylic coatings is 1:4~9.
Preferably, the water-borne acrylic coatings are by mass fraction by 40~70 parts of aqueous acrylic emulsions, 5~10 parts of carbon
Sour calcium, 5~10 parts of mica powders, 1~5 part of defoaming agent, 1~5 part of thickener and 1~20 part of water composition.
Preferably, the water-borne acrylic coatings are by mass fraction by 70 parts of aqueous acrylic emulsions, 5 parts of calcium carbonate, 5 parts
Mica powder, 1 part of defoaming agent, 1 part of thickener and 18 parts of water compositions.
Nanometer heat isolation paint provided by the invention, preparation method includes the following steps:
S10: it is molten by antimony mole doping concentration will to be that 1%~10% weighed stannic chloride pentahydrate and antimony trichloride are dissolved in hydrochloric acid
In liquid, by adding ammonium hydroxide, the first solution that pH value is 9~11 is formed；
S11: first solution is reacted 20~60 minutes under the conditions of being more than or equal to 50 DEG C of water bath with thermostatic control, formed at
It is divided into the first sediment of Sb doped stannic hydroxide；
S15: calcining first sediment obtains antimony doped stannic oxide nano powder；
S20: it by the antimony doped stannic oxide nano powder ultrasonic disperse in dehydrated alcohol, is formed by the way that ammonium hydroxide is added
The second solution that pH value is 9~11；
S21: under agitation, being added ethyl orthosilicate in the second solution of Xiang Suoshu, sufficiently reacts, and is formed with the antimony
Doped stannic oxide nano powder is as the first kernel, the second sediment of external sheath Silicon dioxide, hydrate；
S25: calcining second sediment obtains the intermediate powder of the first kernel described in coated with silica；
S30: stannic chloride pentahydrate and antimony trichloride are dissolved into containing levulinic for 5%~15% by antimony mole doping concentration
In the dehydrated alcohol of ketone, sufficiently reaction is stirred, forms third solution, then distilled water is slowly added dropwise into the third solution, institute
The volume ratio for stating distillation water consumption and the dehydrated alcohol dosage is that 1.4~1.8:100 is displayed after continuing stirring 1~2 hour
Aging obtains Sb doped stannic hydroxide colloidal sol；
S31: the intermediate powder is added to the Sb doped stannic hydroxide colloidal sol by the mass volume ratio of 2g/100ml
In and carry out ultrasonic disperse, then sealing and standing is formed using the intermediate powder as the second kernel, external sheath Sb doped hydrogen
The third sediment of tin oxide；
S35: it dries, calcine the third sediment and obtain nano antimony-doped tin dioxide and coat second kernel being formed
Compound nuclear shell structure nano powder；
S40: 4~9 parts aqueous third are added using 1 part of compound nuclear shell structure nano powder as additive by mass fraction
In olefin(e) acid coating；
S45: ultrasonic disperse makes the compound nuclear shell structure nano powder be dispersed in the water-borne acrylic coatings
In, form nanometer heat isolation paint.
Preferably, in step slo, the molar concentration of the hydrochloric acid solution is 1~3mol/L.
Preferably, in step S10 and S20, the volumetric concentration of the ammonium hydroxide is 10%~30%.
Preferably, in step S31, the ultrasonic disperse time is 15~30 minutes, and the sealing and standing time is 16~32 small
When.
Preferably, in step S15, S25 and S35, the temperature of the calcining is 500~800 DEG C, and calcination time is 1~3
Hour.
It preferably, further include being filtered, washing to first sediment before calcination between step S11 and S15
The step of with drying.
It preferably, further include being filtered, washing to second sediment before calcination between step S21 and S25
The step of with drying.
It preferably, further include being filtered, washing to the third sediment before calcination between step S31 and S35
The step of with drying.
Preferably, in step S40, the water-borne acrylic coatings are by mass fraction by 40~70 portions of aqueous acrylamide yogurts
Liquid, 5~10 parts of calcium carbonate, 5~10 parts of mica powders, 1~5 part of defoaming agent, 1~5 part of thickener and 1~20 part of water composition.
Preferably, in step S45, the time of the ultrasonic disperse is 15~30 minutes.
The invention has the benefit that nanometer heat isolation paint provided by the invention, adds tool in water-borne acrylic coatings
There is the compound nuclear shell structure nano powder of good heat-proof quality to form.The compound nuclear shell structure nano powder passes through in nanometer antimony
Doping stannic oxide particle surface coats layer of silicon dioxide as intermediate medium, then coats one layer of nano antimony-doped dioxy again
Change tin, prepares NEW TYPE OF COMPOSITE core-shell structure nanopowder composite material for nanometer heat isolation paint, production equipment and process side
Method is simple, and economic cost is low.The insulating moulding coating with compound nuclear shell structure nano powder that this method is prepared, the dispersion of powder
Property than using the insulating moulding coating of antimony doped stannic oxide nanometer material good merely, heat insulation is also more preferably.
Detailed description of the invention
Fig. 1 is 6,000 times of SEM photographs of No. 1 nano material sample；
Fig. 2 is 10,000 times of SEM photographs of No. 1 nano material sample；
Fig. 3 is 6,000 times of SEM photographs of No. 2 nano material samples；
Fig. 4 is 10,000 times of SEM photographs of No. 2 nano material samples；
Fig. 5 is 6,000 times of SEM photographs of No. 3 nano material samples；
Fig. 6 is 10,000 times of SEM photographs of No. 3 nano material samples；
Fig. 7 is the diffracted intensity curve comparison figure of 1 to No. 6 nano material sample；
Fig. 8 is warm in the case for being thermally shielded test after the aluminium sheet covering bubble chamber of 0 to No. 6 nanometer heat isolation paint using being coated with
Spend change curve comparison diagram.
Specific embodiment
Below by specific embodiment to further illustrate the technical scheme of the present invention.
Embodiment one
A kind of nanometer heat isolation paint provided in this embodiment, water-borne acrylic coatings and makes an addition to the water soluble acrylic acid
Compound nuclear shell structure nano powder in coating, the compound nuclear shell structure nano powder include: the first kernel, in described first
Core is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 8.5%；Middle layer, the middle layer is is coated on
The silicon dioxide layer outside the first kernel is stated, first kernel and middle layer constitute intermediate powder；Outer layer, the outer layer are cladding
The antimony doped stannic oxide nano powder layer for being 10% in the antimony mole doping concentration outside the intermediate powder；The aqueous acrylamide
Sour coating (hereinafter referred to as No. 0 nanometer heat isolation paint) is by mass fraction by 70 parts of aqueous acrylic emulsions, 5 parts of calcium carbonate, 5 parts of clouds
Female powder, 1 part of defoaming agent, 1 part of thickener and 18 parts of water compositions.
A kind of nanometer heat isolation paint provided in this embodiment, preparation method includes the following steps:
S10: 33g stannic chloride pentahydrate will be weighed for 8.5% by antimony mole doping concentration and 2g antimony trichloride is dissolved in 2mol/L
Hydrochloric acid solution in, by addition volumetric concentration be 10% ammonium hydroxide, form the first solution of pH=9；
S11: first solution is reacted 30 minutes under the conditions of 60 DEG C of water bath with thermostatic control, and forming component is Sb doped hydrogen
Tin oxide (Sn (OH)4·Sb(OH)3) the first sediment of yellow, reaction equation is as follows:
SnCl4·5H2O+SbCl3+NH3·H2O→Sn(OH)4·Sb(OH)3↓+NH4Cl；
S12: it filters first solution and obtains first sediment；
S13: obtained the first sediment ethyl alcohol will be filtered and deionized water is respectively washed 5 times；
S14: first sediment after cleaning is dried 12 hours at 80 DEG C；
S15: first sediment after cleaning is put into Muffle furnace and is calcined 2 hours at 650 DEG C, to the Sb doped hydrogen
Tin oxide is dehydrated, and after natural cooling, obtains navy blue antimony doped stannic oxide nano powder, by the Sb doped dioxy
Change tin nano-powder and be scanned electron microscope (SEM) shooting as No. 1 nano material sample, wherein 6,000 times of SEM photographs
As shown in Figure 1,10,000 times of SEM photographs are as shown in Fig. 2, by Fig. 1~2 it is found that being mixed using the antimony of above-mentioned coprecipitation synthesis
The pattern of miscellaneous stannic oxide nano powder is the block of size unevenness；
S20: the navy blue antimony doped stannic oxide nano powder is added in the dehydrated alcohol of 100ml, ultrasound point
It dissipates 30 minutes, it is the second solution that 10% ammonium hydroxide forms that pH value is 9 that volumetric concentration, which is then added, is stirred 30 minutes；
S21: under agitation, being added ethyl orthosilicate 20ml, sufficiently reaction 3.5 hours in the second solution of Xiang Suoshu,
It is formed using the antimony doped stannic oxide nano powder as the first kernel, the second precipitating of external sheath Silicon dioxide, hydrate
Object；
S22: it filters second solution and obtains second sediment；
S23: obtained the second sediment ethyl alcohol will be filtered and deionized water is respectively washed 5 times；
S24: second sediment after cleaning is dried 12 hours at 80 DEG C；
S25: second sediment after cleaning is put into Muffle furnace and calcines 2 hours to the external sheath at 650 DEG C
Silicon dioxide, hydrate be dehydrated, after natural cooling, obtain the first kernel as described in coated with silica of light slate gray
The intermediate powder of formation；The intermediate powder is scanned electron microscope (SEM) shooting as No. 2 nano material samples,
Wherein 6,000 times of SEM photographs as shown in figure 3,10,000 times of SEM photographs as shown in figure 4, by Fig. 3~4 it is found that being coated with silica
The particle sizes of namely No. 2 nano material samples of antimony doped stannic oxide nano powder obviously become smaller, distribution is also compared
Uniformly, pattern structure spherical in shape, average grain diameter are respectively less than 0.3 μm；
S30: by will be that 10% weigh 30g stannic chloride pentahydrate and 2.17g antimony trichloride is dissolved by antimony mole doping concentration
In the mixed solution of 8ml acetylacetone,2,4-pentanedione and 100ml dehydrated alcohol, first ultrasonic disperse 15 minutes, then magnetic agitation 30 minutes, shape
1.6ml distilled water is slowly added dropwise at the clear third solution of clear, yellowish, then into the third solution, it is small to continue stirring 1
Shi Hou after displaying aging 24 hours, obtains Sb doped stannic hydroxide colloidal sol；
S31: the intermediate powder for weighing 1.0g light slate gray is added in Sb doped stannic hydroxide colloidal sol described in 50ml,
Ultrasonic disperse 15 minutes, then sealing and standing 24 hours, formed using the intermediate powder as the second kernel, external sheath antimony is mixed
The third sediment of miscellaneous stannic hydroxide；
S32: it filters the Sb doped stannic hydroxide colloidal sol and obtains the third sediment；
S33: the obtained third sediment will be filtered and cleaned 5 times with ethyl alcohol；
S34: the third sediment after cleaning is dried 12 hours at 80 DEG C；
S35: the third sediment after cleaning is put into Muffle furnace and calcines 2 hours to the external sheath at 650 DEG C
Sb doped stannic hydroxide be dehydrated, after natural cooling, obtain nano antimony-doped tin dioxide cladding described second in karyomorphism
At compound nuclear shell structure nano powder, the compound nuclear shell structure nano powder is swept as No. 3 nano material samples
Electron microscope (SEM) shooting is retouched, wherein 6,000 times of SEM photographs are as shown in figure 5,10,000 times of SEM photographs are as shown in Figure 6；By Fig. 5
~6 it is found that No. 3 nano material samples that antimony mole doping concentration is 10%, powder can be clearly seen that spherical structure, be distributed
Relatively uniform, cladding thickness is larger, this is because the reunion growth of nano surface stibium doping stannic oxide crystallite dimension is related.Its
Size has no and significantly changes compared with No. 2 nano material sample nano-powders；
S40: No. 3 nano material sample 0.2g are weighed and are added as additive in No. 0 nanometer heat isolation paint of 1.8g；
S45: ultrasonic disperse 30 minutes, so that the compound nuclear shell structure nano powder is dispersed in No. 0 heat-insulated painting
In material, No. 3 insulating moulding coatings are formed.
Embodiment two to four
The nanometer heat isolation paint preparation method and embodiment one that embodiment two to four provides are almost the same, with embodiment one
Difference be only that antimony mole doping concentration in step S30 and distillation water consumption, the data comparison of specific Ingredient Amount such as table 1
It is shown.
Each ingredient contrast table in the step S30 of 1 embodiment one to four of table
| Antimony mole doping concentration | Stannic chloride pentahydrate | Antimony trichloride | Dehydrated alcohol | Acetylacetone,2,4-pentanedione | Distilled water | |
| Embodiment one | 10% | 30g | 2.17g | 100ml | 8.0ml | 1.6ml |
| Embodiment two | 5% | 30g | 1.03g | 100ml | 8.0ml | 1.8ml |
| Embodiment three | 7% | 30g | 1.47g | 100ml | 8.0ml | 1.8ml |
| Example IV | 15% | 30g | 3.45g | 100ml | 8.0ml | 1.4ml |
The three kinds of compound nuclear shell structure nanos prepared in the nanometer heat isolation paint preparation method that embodiment two to four provides
Powder is respectively defined as 4 to No. 6 nano material samples secondary.
Embodiment five
The nanometer heat isolation paint preparation method and embodiment one that embodiment five provides are almost the same, the area with embodiment one
It is not only that, embodiment five does not include step S20~S35, and in step s 40 using No. 1 nano material sample replacement described 3
Number nano material sample, finally prepares No. 1 nanometer heat isolation paint.
Embodiment six
The nanometer heat isolation paint preparation method and embodiment one that embodiment six provides are almost the same, the area with embodiment one
It is not only that, embodiment six does not include step S30~S35, and in step s 40 using No. 2 nano material sample replacements described 3
Number nano material sample, finally prepares No. 2 nanometer heat isolation paints.
In order to facilitate comparison various embodiments of the present invention involved in various nano materials, each nano material sample number into spectrum at
Divide corresponding table as shown in table 2, each nanometer heat isolation paint table corresponding with ingredient is as shown in table 3.
2 sample number into spectrum of table table corresponding with ingredient
3 insulating moulding coating sample of table table corresponding with ingredient
Referring to Fig. 7, it is found that 1 to No. 6 each diffraction maximum of nano material sample mentioned in the embodiment of the present invention one to four
Tetragonal phase cassiterite structure (the JCPDS card number: 21~1250, JCPDS:Joint Committee on of data and stannic oxide
Powder Diffraction Standards/ Joint Committee on Powder Diffraction Standards) diffraction maximum it is consistent.There is not antimony
The diffraction maximum of oxide illustrates that all antimony ions enter the tin ion in stannic oxide lattice instead of part.
Compare the diffracted intensity curve of No. 1 and No. 2 nano material sample it can be found that No. 2 nano material samples diffraction
Peak is significantly broadened compared with No. 1 nano material sample, and diffraction peak intensity reduces, and shows the grain size of No. 2 nano material sample powders
It is smaller.The apparent characteristic peak of silica is had no in figure, shows that the silica of cladding is unformed structure and cladding thickness
It is relatively thin.It takes the highest peak of No. 2 nano material samples and No. 1 nano material sample to calculate grain size, is calculated 2 by Scherrer formula
The mean grain size d=2.049nm, the mean grain size d=of No. 1 nano material sample powder of number nano material sample powder
3.919nm.The result shows that after No. 1 nano material coated silica, lighter and crystallite dimension becomes smaller.3~No. 6 nanometers
The diffraction maximum of material sample powder does not change substantially, and crystal is still the stibium doping stannic oxide structure of rutile structure, peak position
Slightly migrate.The diffraction maximum of 3~No. 6 nano material sample powders is more widened compared with No. 2 nano material sample powders have been changed some, is spread out
Penetrate peak intensity reduces slightly.Show that the grain size of 3~No. 6 nano material sample powders is smaller.Take 3~No. 6 nano material samples
Highest peak calculate grain size, the mean grain size d=of No. 3 nano material sample powders is calculated by Scherrer formula
2.115nm, the mean grain size d=1.726nm of No. 4 nano material sample powders, the average crystalline substance of No. 5 nano material sample powders
Granularity 1.741nm, the mean grain size d=2.115nm of No. 6 nano material sample powders, the mean grain size d=of powder
1.856nm.The result shows that with the increase of antimony mole doping concentration in the stibium doping stannic oxide of outermost layer cladding, complex nucleus
The grain size first increases and then decreases of shell structural nano powder.Compare discovery, the grain of sample obtained in the SEM photograph in Fig. 1~6
Diameter calculates resulting crystallite dimension (D much larger than by Scherrer formulaXRD), this is primarily due to DSEMIt is the size of particle, it may
Be by multiple grain colony poly groups at particle, and DXRDIt is single crystallite dimension.
The antimony mole in step S30 is only had adjusted for better contrast and experiment, in the embodiment of the present invention one to four
The dosage of doping concentration and distilled water.Certainly, by experimental verification, in the case where guaranteeing effect of the present invention, the present invention its
In the nanometer heat isolation paint preparation method that his alternate embodiment provides, various reaction conditions and ingredient in each step may be used
To be adjusted in following ratios or range:
S10: stannic chloride pentahydrate and antimony trichloride can be weighed by antimony mole doping concentration for 1%~10%, the hydrochloric acid
The concentration of solution is 1~3mol/L, and the volumetric concentration of ammonium hydroxide is 10%~30%, the pH value of first solution is adjusted to 9~
11；
S11: the temperature of water bath with thermostatic control is 50~90 DEG C, and the reaction time is 20~60 minutes；
S20: the volumetric concentration of ammonium hydroxide is 10%~30%, and the pH value of second solution is 9~11；
S30: stannic chloride pentahydrate and antimony trichloride are weighed for 5%~15% by antimony mole doping concentration, the distilled water is used
The volume ratio of amount and the dehydrated alcohol dosage is 1.4~1.8:100, continues stirring 1~2 hour after distilled water is added；
S31: the ultrasonic disperse time is 15~30 minutes, and the sealing and standing time is 16~32 hours；
S13, S23 and S33: ethyl alcohol wash number is 3~6 times, and deionized water wash number is 0~6 time；
S14, S24 and S34: drying temperature is 70~90 DEG C, and drying time is 10~15 hours；
S15, S25 and S35: calcination temperature range is 500~800 DEG C, and calcination time is 1~3 hour；
S40: No. 3 nano material samples could alternatively be 4 to No. 6 nano materials sample；The nano material
Sample is that 1:4~9 is added in the water-borne acrylic coatings by mass parts ratio；The water-borne acrylic coatings press mass fraction
By 40~70 parts of aqueous acrylic emulsions, 5~10 parts of calcium carbonate, 5~10 parts of mica powders, 1~5 part of defoaming agent, 1~5 part of thickening
Agent and 1~20 part of water composition；
S45: the time of the ultrasonic disperse is 15~30 minutes.
Embodiment seven
For the heat-proof quality of nanometer heat isolation paint that the test embodiment of the present invention one to six provides, by 0 to 6 in the present embodiment
Number nanometer heat isolation paint uniformly brushes the surface of aluminum plate uniform in size respectively, forms a layer thickness as the heat-insulated of 0.5mm
Film, smearing range is full aluminium sheet, is tested for heat-proof quality.Aluminium sheet is having a size of 11.2 × 4.8 × 0.15cm, after film,
It puts and forms 0 to No. 6 aluminum test under room temperature environment after desiccation, do experimental data acquisition for heat-insulated test.
Heat-insulated test:
Experimental situation: indoor test, room temperature: 29 DEG C；
Major experimental stage property: 0 to No. 6 aluminum test, specification is 34 × 25 × 10cm and center of top is provided with 10 × 4cm
Opening bubble chamber, the tengsten lamp of 500W, hygrosensor；
Testing procedure (illustrates) by taking No. 0 aluminum test as an example:
T10: experiment stage property is placed on test wrapper domestic 2 hours, makes the temperature and ambient temperature equilibrium of testing stage property, test
When door and window close, experimental situation wind speed be 0；
T20: being covered on No. 0 aluminum test in the opening of bubble chamber, is aligned with the opening center, to guarantee bubble chamber
Opening is completely covered, and the end of probe of the hygrosensor is set in the bubble chamber for detecting the sky in the bubble chamber
Temperature degree, reading end are set to outside the bubble chamber；
T30: heat source uses the tengsten lamp with 500W similar in solar spectrum, and tengsten lamp is hung over the covering bubble chamber and is opened
Right above No. 0 aluminum test of mouth at 30cm；
T40: start timing when opening tengsten lamp, record the temperature of air in the bubble chamber at intervals of two minutes；To temperature
After degree variation is no more than 0.5 DEG C, (being the 26th minute in the present embodiment) stops recording data as needed.
No. 0 aluminum test is replaced with into 1 to No. 6 aluminum test respectively according to the method described above, obtains and uses 0 to No. 6
Temperature variation data in the bubble chamber that aluminum test is tested forms Fig. 8 with this data creating temperature changing curve diagram.By scheming
8 it is found that under the irradiation of tengsten lamp, and extension at any time, described foam the temperature inside the box rises with it, incipient stage ascensional range
It is larger, it gradually tends to be steady, when irradiating after twenty minutes, air themperature gradually tends to balance in box.Referring to Fig. 8, wherein on to
Aluminium sheet used in the corresponding test of the temperature variation curve of lower arrangement is followed successively by No. 0, No. 1, No. 2, No. 4, No. 5, No. 6 and No. 3 survey
Try aluminium sheet.It can be seen that No. 2 nanometer heat isolation paints, that is, the antimony doped stannic oxide nanometer powder of addition coated silica
The heat insulation of the coating sample of body material and No. 1 nanometer heat isolation paint, that is, addition antimony doped stannic oxide nano powder
The coating sample of material is compared, and heat insulation is preferable；And add the antimony doped stannic oxide nano powder of different Sb doped concentration
Carry out the coating sample of the compound nuclear shell structure nano powder of outermost layer cladding, i.e., the heat insulation of 3 to No. 6 nanometer heat isolation paints
It is superior to No. 1 and No. 2 nanometer heat isolation paints, wherein the heat-proof quality of No. 3 nanometer heat isolation paints is optimal.
In conclusion the nanometer heat isolation paint that the present invention supplies in water-borne acrylic coatings by adding with good heat-insulated
The compound nuclear shell structure nano powder of performance is prepared.The compound nuclear shell structure nano powder passes through in Sb doped titanium dioxide
Tin nano-powder particle surface coats intermediate medium silica, then coats one layer of antimony doped stannic oxide nano powder again.
NEW TYPE OF COMPOSITE core-shell structure nanopowder composite material is prepared for nanometer heat isolation paint, production equipment and process method letter
Single, economic cost is low.By test, additive of the compound nuclear shell structure nano as insulating moulding coating, dispersibility compares antimony
Doped stannic oxide nano powder is more preferably；It can also be verified by above-mentioned experimental result, add the compound core-shell structure nanopowder
The heat-proof quality of heat-barrier material of the heat insulation of the insulating moulding coating of body than adding antimony doped stannic oxide nano powder is more preferable.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of nanometer heat isolation paint, characterized by comprising: water-borne acrylic coatings and make an addition to the water soluble acrylic acid
Compound nuclear shell structure nano powder in coating, the mass parts of compound the nuclear shell structure nano powder and water-borne acrylic coatings
Number is than being 1:4~9；The water-borne acrylic coatings are by mass fraction by 40~70 parts of aqueous acrylic emulsions, 5~10 parts of carbonic acid
Calcium, 5~10 parts of mica powders, 1~5 part of defoaming agent, 1~5 part of thickener and 1~20 part of water composition；The compound core-shell structure is received
Rice flour body includes: the first kernel, and first kernel is that the stibium doping stannic oxide that antimony mole doping concentration is 1%~10% is received
Rice flour body；Middle layer, the middle layer are the silicon dioxide layer being coated on outside first kernel, first kernel and centre
Layer constitutes intermediate powder, and the intermediate powder is as the second kernel；Outer layer, the outer layer are to be coated on outside the intermediate powder
The antimony doped stannic oxide nano powder layer that antimony mole doping concentration is 5%~15%.
2. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that: first kernel is antimony mole doping
The antimony doped stannic oxide nano powder that concentration is 8.5%.
3. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that: the outer layer is to be coated on described second
The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside kernel is 5%.
4. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that: the outer layer is to be coated on described second
The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside kernel is 7%.
5. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that: the outer layer is to be coated on described second
The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside kernel is 10%.
6. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that: the outer layer is to be coated on described second
The antimony doped stannic oxide nano powder layer that antimony mole doping concentration outside core is 15%.
7. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that: the compound nuclear shell structure nano powder
Mean grain size between 1.726nm and 2.115nm.
8. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that: the water-borne acrylic coatings press quality
Number is made of 70 parts of aqueous acrylic emulsions, 5 parts of calcium carbonate, 5 parts of mica powders, 1 part of defoaming agent, 1 part of thickener and 18 parts of water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710487267.1A CN107189583B (en) | 2017-06-23 | 2017-06-23 | A kind of nanometer heat isolation paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710487267.1A CN107189583B (en) | 2017-06-23 | 2017-06-23 | A kind of nanometer heat isolation paint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107189583A CN107189583A (en) | 2017-09-22 |
| CN107189583B true CN107189583B (en) | 2019-05-14 |
Family
ID=59878632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710487267.1A Active CN107189583B (en) | 2017-06-23 | 2017-06-23 | A kind of nanometer heat isolation paint |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107189583B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115820111B (en) * | 2022-10-11 | 2024-03-26 | 航天特种材料及工艺技术研究所 | Ablation-resistant heat-insulating coating, coating and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108946A (en) * | 2007-07-12 | 2008-01-23 | 深圳清华大学研究院 | Nano transparent insulating paint and its preparing process |
| CN103725074A (en) * | 2014-01-06 | 2014-04-16 | 武汉双虎涂料有限公司 | High-temperature-resisting heat-insulation coating as well as preparation method and application thereof |
| CN105457572A (en) * | 2014-09-10 | 2016-04-06 | 北京化工大学 | Silica-coated metal-doped tin oxide material and preparation method thereof, and dispersion body and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101254039B1 (en) * | 2010-12-29 | 2013-04-12 | 전자부품연구원 | Nano particle having multi-layer core-shell of paint for cutting off heat lay |
-
2017
- 2017-06-23 CN CN201710487267.1A patent/CN107189583B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108946A (en) * | 2007-07-12 | 2008-01-23 | 深圳清华大学研究院 | Nano transparent insulating paint and its preparing process |
| CN103725074A (en) * | 2014-01-06 | 2014-04-16 | 武汉双虎涂料有限公司 | High-temperature-resisting heat-insulation coating as well as preparation method and application thereof |
| CN105457572A (en) * | 2014-09-10 | 2016-04-06 | 北京化工大学 | Silica-coated metal-doped tin oxide material and preparation method thereof, and dispersion body and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 纳米ATO水性透明隔热涂料的制备与性能研究;王雅丽 等;《涂料工业》;20141201;第44卷(第12期);第12-18页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107189583A (en) | 2017-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107162044B (en) | A kind of compound nuclear shell structure nano powder preparation method | |
| CN105199435B (en) | A kind of preparation method of cobalt blue/clay mineral hybrid pigment | |
| JP4304343B2 (en) | Zinc oxide fine particles, method for producing aggregates thereof and dispersion solution | |
| CN107140687B (en) | A kind of compound nuclear shell structure nano powder | |
| CN102849962B (en) | Preparation method of SiO2 super-hydrophobic film and super-hydrophobic material | |
| CN106380977A (en) | Hydrophobic heat-insulation coating and preparation method therof | |
| CN1077729A (en) | Conducting pigment | |
| CN106746724B (en) | A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof | |
| CN105347392B (en) | Controllable nano crystalline state TiO2Particle and its preparation method and application | |
| CN102408760B (en) | Heat-insulating coating and preparation method thereof | |
| CN110182834B (en) | Method for preparing flaky alpha-alumina and flaky alpha-alumina | |
| CN108948802A (en) | A kind of automatic cleaning coating of translucency enhancing | |
| CN102329533B (en) | Preparation method of composite tin antimony oxide thermal insulation material | |
| CN107189583B (en) | A kind of nanometer heat isolation paint | |
| CN107267000B (en) | A kind of nanometer heat isolation paint preparation method | |
| CN106629793B (en) | A kind of hollow rodlike MgF2The preparation method of particle and its application in automatically cleaning antireflective film | |
| JPWO2018230472A1 (en) | Method of manufacturing hexagonal plate-like zinc oxide | |
| CN105384176A (en) | Prussian blue composite photonic crystal and preparing method and application thereof | |
| CN102496401B (en) | Light-color electric conduction powder with good thermal insulation and not apt to agglomerate, and preparing method | |
| CN105722903B (en) | Composite pigment | |
| CN106449099B (en) | A kind of preparation method and photo-anode film based on ZnO nano powder photo-anode film | |
| CN109517217A (en) | A kind of tungsten-doped vanadium dioxide/graphene complex and the preparation method and application thereof | |
| CN109535771A (en) | Cobalt blue palygorskite nano composite pigment, preparation method and application | |
| CN115584207A (en) | High-temperature-resistant cooker pigment and preparation method thereof | |
| CN109180220A (en) | A kind of preparation method of photonic crystal structure color glaze |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |