CN107189583A - A kind of nanometer heat isolation paint - Google Patents
A kind of nanometer heat isolation paint Download PDFInfo
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- CN107189583A CN107189583A CN201710487267.1A CN201710487267A CN107189583A CN 107189583 A CN107189583 A CN 107189583A CN 201710487267 A CN201710487267 A CN 201710487267A CN 107189583 A CN107189583 A CN 107189583A
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- 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
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- 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
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- 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
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- 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
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- 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
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Abstract
The invention discloses a kind of nanometer heat isolation paint, it is characterised in that including：Water-borne acrylic coatings and the compound nuclear shell structure nano powder made an addition in the water-borne acrylic coatings, the compound nuclear shell structure nano powder include：First kernel, first kernel is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 1%~10%；Intermediate layer, the intermediate layer is the silicon dioxide layer being coated on outside first kernel, and first kernel and intermediate layer constitute middle powder；Outer layer, the outer layer is the antimony doped stannic oxide nano powder layer that the antimony mole doping concentration being coated on outside the middle powder is 5%~15%.The production equipment and process method of the nanometer heat isolation paint is simple, and financial cost is low.What this method was prepared has the insulating moulding coating of compound nuclear shell structure nano powder, and the dispersiveness of powder is better using the insulating moulding coating of antimony doped stannic oxide nanometer material than simple, and effect of 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 technology
In recent years, hud typed hetero nano structure material due to different from any single substance property materialized
Learn and field of nanometer technology has played extensive concern.Nucleocapsid hetero nano structure material can by different composition functions material structure
Into can build the composite functional material and device of more high-quality by Material cladding, complementary and optimization, meet the demand of development.
In particle surface cladding shell material formation Core-shell structure material, it can be very good to control the interaction between particle, pass through
Particle can be assigned with special functional characteristic by changing the composition of the size, structure and particle of coating, so that it is obtained
More extensive potential application.
Stibium doping stannic oxide (Antimony tin oxide, abbreviation ATO) nano material, while having taken into account ATO materials
With the advantage of nano material, it has unique photoelectric properties, ionizing radiation-resistant, good antireflective, infrared absorption, thermally-stabilised
Property and some members are have with very high ion selectivity exchange capacity, available 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, particularly in Japan, the U.S., the preparation and application study of ATO nano materials 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 materials,
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 materials are a kind of excellent transparent heat-insulated fillers, special with excellent light-coloured transparent and infrared absorption
Property, and corrosion-resistant, heat endurance is high.But, it is desirable to heat-proof quality is further improved, in insulating moulding coating, researcher is by adding
Plus a certain amount of inorganic nano-particle is modified to coating property.For example, Publication No. CN1563231A Chinese invention
Patent discloses one kind nano ATO wet pulp and nano-indium stannum oxide (Indium Tin Oxide, abbreviation ITO) wet pulp as changing
Property filler is added in glass coating so that coating has good visible light transmissivity and very high infrared shielding effect.And
Nano-glass heat insulation paint need to only brush several microns of thickness, it is possible to reach very excellent effect of heat insulation, easy to operate
And it is cheap.ATO nano-particles have a good antireflective in itself, the function such as radioresistance and infrared absorption, and it is good
Light transmittance, weatherability and stability, and its cheap cost so that it turns into the nanometer of the nanometer heat isolation paint of present main flow
Filler.It is saturating that Publication No. CN106118287A Chinese invention patent discloses a kind of nano ATO/CuS filler water soluble acrylic acids
It is bright heat-insulated, filled using nano ATO/CuS mixing, reach the purpose of improving performance.
The content of the invention
In order to overcome the defect of prior art, the present invention proposes a kind of nanometer heat isolation paint.
For up to this purpose, a kind of nanometer heat isolation paint that the present invention is provided, including：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 is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 1%~10%；Intermediate layer,
The intermediate layer is the silicon dioxide layer being coated on outside first kernel, and first kernel and intermediate layer constitute middle powder
Body；Outer layer, the outer layer is the Sb doped dioxy that the antimony mole doping concentration being coated on outside the middle powder is 5%~15%
Change tin nano-powder layer.
It is preferred that, first kernel is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 8.5%.
It is preferred that, 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.
It is preferred that, 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.
It is preferred that, 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.
It is preferred that, 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.
It is preferred that, the mean grain size of the compound nuclear shell structure nano powder is between 1.726nm and 2.115nm.
It is preferred that, the quality parts ratio of compound the nuclear shell structure nano powder and water-borne acrylic coatings is 1：4~9.
It is preferred that, 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 defoamer, 1~5 part of thickener and 1~20 part of water composition.
It is preferred that, the water-borne acrylic coatings by mass fraction by 70 parts of aqueous acrylic emulsions, 5 parts of calcium carbonate, 5 parts
Mica powder, 1 part of defoamer, 1 part of thickener and 18 parts of water compositions.
The nanometer heat isolation paint that the present invention is provided, its preparation method comprises the following steps：
S10：It is molten by being that 1%~10% five water stannic chlorides weighed and trichloride antimony are dissolved in hydrochloric acid by antimony mole doping concentration
In liquid, by adding ammoniacal liquor, the first solution that pH value is 9~11 is formed；
S11：First solution is reacted 20~60 minutes under the conditions of the water bath with thermostatic control more than or equal to 50 DEG C, formed into
It is divided into the first sediment of Sb doped stannic hydroxide；
S15：First sediment is calcined, antimony doped stannic oxide nano powder is obtained；
S20：By the antimony doped stannic oxide nano powder ultrasonic disperse in absolute ethyl alcohol, formed by adding ammoniacal liquor
PH value is 9~11 the second solution；
S21：Under agitation, tetraethyl orthosilicate is added into second solution, fully reaction, is formed with the antimony
Doped stannic oxide nano powder is used as the first kernel, the second sediment of external sheath Silicon dioxide, hydrate；
S25：Second sediment is calcined, the middle powder of the first kernel described in coated with silica is obtained；
S30：Five water stannic chlorides and trichloride antimony are dissolved into containing levulinic for 5%~15% by antimony mole doping concentration
In the absolute ethyl alcohol of ketone, stirring fully reaction forms the 3rd solution, then distilled water is slowly added dropwise into the 3rd solution, institute
The volume ratio for stating distillation water consumption and the absolute ethyl alcohol consumption is 1.4~1.8:100, continue after stirring 1~2 hour, display
Aging obtains Sb doped stannic hydroxide colloidal sol；
S31：The middle powder is added to the Sb doped stannic hydroxide colloidal sol by 2g/100ml mass volume ratio
In and carry out ultrasonic disperse, then sealing and standing is formed using the middle powder as the second kernel, external sheath Sb doped hydrogen
3rd sediment of tin oxide；
S35：Dry, calcine the 3rd sediment and obtain nano antimony-doped tin dioxide and coat second kernel being formed
Compound nuclear shell structure nano powder；
S40：By mass fraction 4~9 parts aqueous third are added using 1 part of compound nuclear shell structure nano powder as additive
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.
It is preferred that, in step slo, the molar concentration of the hydrochloric acid solution is 1~3mol/L.
It is preferred that, in step S10 and S20, the volumetric concentration of the ammoniacal liquor is 10%~30%.
It is preferred that, in step S31, the ultrasonic disperse time is 15~30 minutes, and the sealing and standing time is 16~32 small
When.
It is preferred that, in step S15, S25 and S35, the temperature of the calcining is 500~800 DEG C, and calcination time is 1~3
Hour.
It is preferred that, between step S11 and S15, first sediment is filtered, washed before being additionally included in calcining
The step of with drying.
It is preferred that, between step S21 and S25, second sediment is filtered, washed before being additionally included in calcining
The step of with drying.
It is preferred that, between step S31 and S35, the 3rd sediment is filtered, washed before being additionally included in calcining
The step of with drying.
It is preferred that, 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 defoamer, 1~5 part of thickener and 1~20 part of water composition.
It is preferred that, in step S45, the time of the ultrasonic disperse is 15~30 minutes.
Beneficial effects of the present invention are：The nanometer heat isolation paint that the present invention is provided, adds tool in water-borne acrylic coatings
The compound nuclear shell structure nano powder for having good heat-proof quality is formed.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, and one layer of nano antimony-doped dioxy is then coated again
Change tin, preparing NEW TYPE OF COMPOSITE core-shell structure nanopowder composite material is used for nanometer heat isolation paint, production equipment and process side
Method is simple, and financial cost is low.What this method was prepared the have insulating moulding coating of compound nuclear shell structure nano powder, powder it is scattered
Property it is better using the insulating moulding coating of antimony doped stannic oxide nanometer material than simple, effect of heat insulation is also more preferably.
Brief description of the drawings
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 using being thermally shielded after the aluminium sheet covering bubble chamber for scribbling 0 to No. 6 nanometer heat isolation paint in the case of test
Spend change curve comparison diagram.
Embodiment
Technical scheme is further illustrated below by specific embodiment.
Embodiment one
A kind of nanometer heat isolation paint that the present embodiment is provided, 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 includes：First kernel, in described first
Core is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 8.5%；Intermediate layer, the intermediate layer is is coated on
The silicon dioxide layer outside the first kernel is stated, first kernel and intermediate layer constitute middle powder；Outer layer, the outer layer is cladding
In the antimony doped stannic oxide nano powder layer that the antimony mole doping concentration outside the middle powder is 10%；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 defoamer, 1 part of thickener and 18 parts of water compositions.
A kind of nanometer heat isolation paint that the present embodiment is provided, its preparation method comprises the following steps：
S10：The water stannic chlorides of 33g five will be weighed for 8.5% and 2g trichloride antimonies are dissolved in 2mol/L by antimony mole doping concentration
Hydrochloric acid solution in, by adding volumetric concentration for 10% ammoniacal liquor, form pH=9 the first solution；
S11：First solution is reacted 30 minutes under the conditions of 60 DEG C of water bath with thermostatic control, forming component is Sb doped hydrogen
Tin oxide (Sn (OH)4·Sb(OH)3) the sediment of yellow first, reaction equation is as follows:
SnCl4·5H2O+SbCl3+NH3·H2O→Sn(OH)4·Sb(OH)3↓+NH4Cl；
S12：First solution described in suction filtration obtains first sediment；
S13：First sediment that suction filtration is obtained is respectively washed 5 times with ethanol and deionized water；
S14：First sediment after cleaning is dried 12 hours at 80 DEG C；
S15：First sediment after cleaning is put into Muffle furnace to calcine 2 hours at 650 DEG C, to the Sb doped hydrogen
Tin oxide is dehydrated, 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 using the antimony of above-mentioned coprecipitation synthesis as shown in Fig. 2 from Fig. 1~2, mixed
The pattern of miscellaneous stannic oxide nano powder is the uneven block of size；
S20：The navy blue antimony doped stannic oxide nano powder is added in 100ml absolute ethyl alcohol, ultrasound point
Dissipate 30 minutes, it is the second solution that 10% ammoniacal liquor formation pH value is 9 then to add volumetric concentration, is stirred 30 minutes；
S21：Under agitation, tetraethyl orthosilicate 20ml, fully reaction 3.5 hours are added into second solution,
Formed using the antimony doped stannic oxide nano powder as the first kernel, the second precipitation of external sheath Silicon dioxide, hydrate
Thing；
S22：Second solution described in suction filtration obtains second sediment；
S23：Second sediment that suction filtration is obtained is respectively washed 5 times with ethanol and deionized water；
S24：Second sediment after cleaning is dried 12 hours at 80 DEG C；
S25：Second sediment after cleaning is put into Muffle furnace 2 hours are calcined at 650 DEG C to the external sheath
Silicon dioxide, hydrate be dehydrated, after natural cooling, obtain the first kernel as described in coated with silica of light slate gray
The middle powder of formation；The middle powder is scanned into electron microscope (SEM) as No. 2 nano material samples to shoot,
Wherein 6,000 times SEM photographs are as shown in figure 3,10,000 times of SEM photographs are as shown in figure 4, from Fig. 3~4, be coated with silica
The particle sizes of namely No. 2 nano material samples of antimony doped stannic oxide nano powder substantially diminish, distribution is also compared
Uniformly, pattern structure spherical in shape, average grain diameter is respectively less than 0.3 μm；
S30：By will be that 10% weigh the water stannic chlorides of 30g five and 2.17g trichloride antimonies are dissolved into by antimony mole doping concentration
In the mixed solution of 8ml acetylacetone,2,4-pentanediones and 100ml absolute ethyl alcohols, first ultrasonic disperse 15 minutes, then magnetic agitation 30 minutes, shape
The 3rd solution clarified into clear, yellowish, then 1.6ml distilled water is slowly added dropwise into the 3rd solution, continue stirring 1 small
Shi Hou, after displaying aging 24 hours, obtains Sb doped stannic hydroxide colloidal sol；
S31：The middle powder for weighing 1.0g light slate grays is added in Sb doped stannic hydroxide colloidal sol described in 50ml,
Ultrasonic disperse 15 minutes, then sealing and standing 24 hours, are formed using the middle powder as the second kernel, external sheath antimony is mixed
3rd sediment of miscellaneous stannic hydroxide；
S32：Sb doped stannic hydroxide colloidal sol obtains the 3rd sediment described in suction filtration；
S33：The 3rd sediment that suction filtration is obtained is cleaned 5 times with ethanol；
S34：The 3rd sediment after cleaning is dried 12 hours at 80 DEG C；
S35：The 3rd sediment after cleaning is put into Muffle furnace 2 hours are calcined at 650 DEG C to the external sheath
Sb doped stannic hydroxide be dehydrated, after natural cooling, obtain nano antimony-doped tin dioxide cladding described second in karyomorphism
Into 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 understand, antimony mole doping concentration is 10% No. 3 nano material samples, and its powder can be clearly seen that spherical structure, are distributed
Than more uniform, cladding thickness is larger, this be due to nano surface stibium doping stannic oxide crystallite dimension reunion growth it is relevant.Its
Size has no and significantly changed compared with No. 2 nano material sample nano-powders；
S40：No. 3 nano material sample 0.2g are weighed to add as additive in 1.8g No. 0 nanometer heat isolation paint；
S45：Ultrasonic disperse 30 minutes, makes the compound nuclear shell structure nano powder be dispersed in described 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 is provided are basically identical, itself and embodiment one
The antimony mole doping concentration differed only in step S30 and distillation water consumption, the data comparison such as table 1 of specific Ingredient Amount
It is shown.
Each composition contrast table in the step S30 of the embodiment one to four of table 1
| Antimony mole doping concentration | Five water stannic chlorides | Trichloride antimony | Absolute ethyl 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 is provided
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 is provided are basically identical, its area with embodiment one
It is not only that, embodiment five does not include step S20~S35, and replaces described 3 using No. 1 nano material sample in step s 40
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 is provided are basically identical, its area with embodiment one
It is not only that, embodiment six does not include step S30~S35, and replaces described 3 using No. 2 nano material samples in step s 40
Number nano material sample, finally prepares No. 2 nanometer heat isolation paints.
The various nano materials that are related in contrast various embodiments of the present invention for convenience, each nano material sample number into spectrum with into
Divide corresponding table as shown in table 2, each nanometer heat isolation paint and composition corresponding table are as shown in table 3.
The sample number into spectrum of table 2 and composition corresponding table
The insulating moulding coating sample of table 3 and composition corresponding table
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 cassiterite structure (the JCPDS card numbers of data and tin ash：21~1250, JCPDS：Joint Committee on
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 that part is instead of in tin ash lattice.
Compare the diffracted intensity curve of No. 1 and No. 2 nano material sample it can be found that the diffraction of No. 2 nano material samples
Peak shows the grain size of No. 2 nano material sample powders compared with significantly broadened, the diffraction peak intensity reduction of No. 1 nano material sample
It is smaller.The obvious characteristic peak of silica is had no in figure, it is unformed structure and cladding thickness to show the silica of cladding
It is relatively thin.Take the highest peak of No. 2 nano material samples and No. 1 nano material sample to calculate grain size, 2 are calculated 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.As a result show, after No. 1 nano material coated silica, lighter and crystallite dimension diminishes.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 and has 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.As a result show, the increase of antimony mole doping concentration, complex nucleus in the stibium doping stannic oxide coated with outermost layer
The grain size first increases and then decreases of shell structural nano powder.The grain of the sample obtained in SEM photograph in contrast discovery, Fig. 1~6
Footpath, much larger than as the crystallite dimension (D obtained by the calculating of Scherrer formulaXRD), this is primarily due to DSEMIt is the size of particle, it may
The particle being made up of the reunion of multiple crystal grain, and DXRDIt is single crystallite dimension.
The antimony mole in step S30 is only have adjusted for more preferable contrast and experiment, in the embodiment of the present invention one to four
The consumption of doping concentration and distilled water.Certainly, by experimental verification, in the case where ensureing effect of the present invention, it is of the invention its
In the nanometer heat isolation paint preparation method that his alternate embodiment is provided, various reaction conditions and composition also may be used in each step
To be adjusted in following ratios or scope：
S10：Five water stannic chlorides and trichloride antimony 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 ammoniacal liquor 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 ammoniacal liquor is 10%~30%, and the pH value of second solution is 9~11；
S30：Five water stannic chlorides and trichloride antimony are weighed for 5%~15% by antimony mole doping concentration, the distilled water is used
Amount and the volume ratio of the absolute ethyl alcohol consumption are 1.4~1.8:100, add after distilled water and continue to stir 1~2 hour；
S31：The ultrasonic disperse time is 15~30 minutes, and the sealing and standing time is 16~32 hours；
S13, S23 and S33：Ethanol 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 1 by quality parts ratio：4~9 add in the water-borne acrylic coatings；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 defoamer, 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
By 0 to 6 in the heat-proof quality of the nanometer heat isolation paint provided for the test embodiment of the present invention one to six, the present embodiment
Number nanometer heat isolation paint is uniform respectively to be brushed in the homogeneous surface of aluminum plate of size, and it is the heat-insulated of 0.5mm to form a layer thickness
Film, it is full aluminium sheet to smear scope, for heat-proof quality test.Aluminium sheet size is 11.2 × 4.8 × 0.15cm, after film,
Put and form 0 to No. 6 aluminum test under room temperature environment after desiccation, experimental data collection is done for heat-insulated test.
Heat-insulated test：
Experimental situation：Indoor test, room temperature：29℃；
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, 500W tengsten lamp, hygrosensor；
Testing procedure (illustrates) by taking No. 0 aluminum test as an example：
T10：Experiment stage property is placed in test environment 2 hours, makes the temperature and ambient temperature equilibrium of test stage property, is tested
When door and window close, experimental situation wind speed be 0；
T20：No. 0 aluminum test is covered in the opening of bubble chamber, and the opening center alignment, to ensure bubble chamber
Opening is completely covered, and the end of probe of the hygrosensor is used to detect the sky in the bubble chamber in the bubble chamber
Temperature degree, reading end is outside the bubble chamber；
T30：Thermal source uses the 500W close with solar spectrum tengsten lamp, and tengsten lamp, which is hung over the covering bubble chamber, to be opened
Directly over No. 0 aluminum test of mouth at 30cm；
T40：Start timing when opening tengsten lamp, the temperature of air in the bubble chamber is recorded at intervals of two minutes；To temperature
Degree change is no more than after 0.5 DEG C, as needed (being the 26th minute in the present embodiment) stop recording data.
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, Fig. 8 is formed with this data creating temperature changing curve diagram.By scheming
8 understand that under the irradiation of tengsten lamp, with the extension of time, described foam the temperature inside the box rises therewith, incipient stage ascensional range
It is larger, gradually tend to be steady, after irradiating 20 minutes, air themperature gradually tends to balance in box.Referring to Fig. 8, wherein on to
Aluminium sheet used in the temperature variation curve correspondence test 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.As can be seen here, No. 2 nanometer heat isolation paints, that is, add the antimony doped stannic oxide nanometer powder of coated silica
The effect of heat insulation of the coating sample of body material and No. 1 nanometer heat isolation paint, that is, add antimony doped stannic oxide nano powder
The coating sample of material is compared, and effect of 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 effect of heat insulation of 3 to No. 6 nanometer heat isolation paints
No. 1 and No. 2 nanometer heat isolation paints are superior to, wherein, the heat-proof quality of No. 3 nanometer heat isolation paints is optimal.
In summary, the nanometer heat isolation paint that the present invention is supplied in water-borne acrylic coatings by adding with good heat-insulated
The compound nuclear shell structure nano powder of performance is prepared from.The compound nuclear shell structure nano powder passes through in Sb doped titanium dioxide
Tin nano-powder particle surface coats intermediate medium silica, and one layer of antimony doped stannic oxide nano powder is then coated again.
Preparing NEW TYPE OF COMPOSITE core-shell structure nanopowder composite material is used for nanometer heat isolation paint, the letter of production equipment and process method
Single, financial cost is low.By test, the compound nuclear shell structure nano is as the additive of insulating moulding coating, and its dispersiveness 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 effect of 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 the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of 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, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It may be appreciated other embodiment.
Claims (10)
1. a kind of nanometer heat isolation paint, it is characterised in that including：Water-borne acrylic coatings and make an addition to the water soluble acrylic acid
Compound nuclear shell structure nano powder in coating, the compound nuclear shell structure nano powder includes：First kernel, in described first
Core is the antimony doped stannic oxide nano powder that antimony mole doping concentration is 1%~10%；Intermediate layer, the intermediate layer is cladding
Silicon dioxide layer outside first kernel, first kernel and intermediate layer constitute middle powder；Outer layer, the outer layer is
It is 5%~15% antimony doped stannic oxide nano powder layer to be coated on the antimony mole doping concentration outside the middle powder.
2. a kind of nanometer heat isolation paint according to claim 1, it is characterised in that：First kernel adulterates for antimony mole
Concentration is 8.5% antimony doped stannic oxide nano powder.
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 kernel 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 any one in claim 1~7, it is characterised in that：The complex nucleus
The quality parts ratio of shell structural nano powder and water-borne acrylic coatings is 1：4~9.
9. a kind of nanometer heat isolation paint according to claim 8, it is characterised in that：The water-borne acrylic coatings press quality
Number by 40~70 parts of aqueous acrylic emulsions, 5~10 parts of calcium carbonate, 5~10 parts of mica powders, 1~5 part of defoamer, 1~5 part
Thickener and 1~20 part of water composition.
10. a kind of nanometer heat isolation paint according to claim 9, it is characterised in that：The water-borne acrylic coatings press matter
Number is measured by 70 parts of aqueous acrylic emulsions, 5 parts of calcium carbonate, 5 parts of mica powders, 1 part of defoamer, 1 part of thickener and 18 parts of water groups
Into.
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| CN115820111A (en) * | 2022-10-11 | 2023-03-21 | 航天特种材料及工艺技术研究所 | Ablation-resistant heat-insulating coating, coating and preparation method thereof |
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| 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 |
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