CN107267000B

CN107267000B - A kind of nanometer heat isolation paint preparation method

Info

Publication number: CN107267000B
Application number: CN201710488219.4A
Authority: CN
Inventors: 杨波; 李茂东; 黄国家; 常萌蕾; 张双红; 王志刚; 李仕平; 翟伟; 伍振凌; 何颖怡; 常亮; 潘莹
Original assignee: Guangzhou Special Pressure Equipment Inspection and Research Institute
Current assignee: Guangzhou Special Pressure Equipment Inspection and Research Institute
Priority date: 2017-06-23
Filing date: 2017-06-23
Publication date: 2019-05-14
Anticipated expiration: 2037-06-23
Also published as: CN107267000A

Abstract

The invention discloses a kind of nanometer heat isolation paint preparation methods, comprising the following steps: stannic chloride pentahydrate and antimony trichloride is dissolved in hydrochloric acid solution, addition ammonium hydroxide forms the first solution；First solution is reacted under the conditions of water bath with thermostatic control, the first sediment is formed, obtains antimony doped stannic oxide nano powder after calcining；It disperses the antimony doped stannic oxide nano powder in dehydrated alcohol, addition ammonium hydroxide forms the second solution；Ethyl orthosilicate is added to second solution to react to form the second sediment, intermediate powder is obtained after calcining；Stannic chloride pentahydrate and antimony trichloride are dissolved into the dehydrated alcohol containing acetylacetone,2,4-pentanedione, are stirred to react, third solution is formed, after distilled water stirring is added dropwise, aging is displayed and obtains Sb doped stannic hydroxide colloidal sol；The intermediate powder is added in the Sb doped stannic hydroxide colloidal sol and is dispersed, then sealing and standing, third sediment is formed, after calcining, obtains compound nuclear shell structure nano powder；It disperses compound nuclear shell structure nano powder in water-borne acrylic coatings, forms nanometer heat isolation paint.

Description

A kind of nanometer heat isolation paint preparation method

Technical field

The present invention relates to a kind of method for preparing insulating mold coating, especially a kind of nanometer heat isolation paint preparation method.

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 preparation method.

For this purpose, a kind of nanometer heat isolation paint preparation method provided by the invention, comprising 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 preparation method provided by the invention using chemical coprecipitation with The method that sol-gal process combines, by being coated in layer of silicon dioxide conduct in nano antimony-doped tin dioxide particle surface Between medium, then coat one layer of nano antimony-doped tin dioxide again, prepare NEW TYPE OF COMPOSITE core-shell structure nanopowder bluk recombination material Material is used for nanometer heat isolation paint, and experimental facilities and process are simple, and economic cost is low.What this method was prepared has complex nucleus The insulating moulding coating of shell structural nano powder, the dispersibility of powder is than the simple heat-insulated painting for using antimony doped stannic oxide nanometer material Expect, 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 preparation method provided in this embodiment, comprising 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: weighing No. 3 nano material sample 0.2g and be added in No. 0 nanometer heat isolation paint of 1.8g as additive, Wherein No. 0 nanometer heat isolation paint uses water-borne acrylic coatings, and the water-borne acrylic coatings are by mass fraction by 70 parts Aqueous acrylic emulsion, 5 parts of calcium carbonate, 5 parts of mica powders, 1 part of defoaming agent, 1 part of thickener and 18 parts of water compositions；

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 nanometer heat isolation paint 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 formula_XRD), this is primarily due to D_SEMIt is the size of particle, it may Be by multiple grain colony poly groups at particle, and D_XRDIt 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 nanometer heat isolation paint for the nanometer heat isolation paint preparation method preparation that the test embodiment of the present invention one to six provides Heat-proof quality, 0 to No. 6 nanometer heat isolation paint is uniformly brushed into the aluminium sheet table uniform in size respectively in the present embodiment Face forms the heat insulating coating film that a layer thickness is 0.5mm, and smearing range is full aluminium sheet, is tested for heat-proof quality.Aluminium sheet size For 11.2 × 4.8 × 0.15cm, after film, puts and form 0 to No. 6 aluminum test under room temperature environment after desiccation, be used for heat-insulated test Do experimental data acquisition.

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 nanometer heat isolation paint of body material and No. 1 nanometer heat isolation paint, that is, addition antimony doped stannic oxide nanometer The nanometer heat isolation paint of powder body material is compared, and heat insulation is preferable；And add the stibium doping stannic oxide of different Sb doped concentration Nano-powder carries out the nanometer heat isolation paint of the compound nuclear shell structure nano powder of outermost layer cladding, i.e. 3 to No. 6 nano heat-insulatings apply The heat insulation of material 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 preparation method that the present invention supplies is using chemical coprecipitation and sol-gal process phase In conjunction with method, by antimony doped stannic oxide nano powder particle surface coat intermediate medium silica, then wrap again One layer of antimony doped stannic oxide nano powder is covered, NEW TYPE OF COMPOSITE core-shell structure nanopowder body, Preparation equipment and technique side are prepared Method is simple, and economic cost is low.By test, additive of the compound nuclear shell structure nano as insulating moulding coating, dispersibility More preferably than antimony doped stannic oxide nano powder；It can also be verified by above-mentioned experimental result, add the compound core-shell structure and receive The heat-proof quality of heat-barrier material of the heat insulation of the insulating moulding coating of rice flour body than adding antimony doped stannic oxide nano powder is more It is good.

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

1. a kind of nanometer heat isolation paint preparation method, it is characterised in that the following steps are included:

S10: will be that 1%~10% weighed stannic chloride pentahydrate and antimony trichloride are dissolved in hydrochloric acid solution by antimony mole doping concentration In, by adding ammonium hydroxide, form the first solution that pH value is 9~11；

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, forming component is First sediment of Sb doped stannic hydroxide；

S20: by the antimony doped stannic oxide nano powder ultrasonic disperse in dehydrated alcohol, pH value is formed by the way that ammonium hydroxide is added For 9~11 the second solution；

S21: under agitation, being added ethyl orthosilicate in the second solution of Xiang Suoshu, sufficiently reacts, and is formed with the Sb doped Stannic oxide nano powder is as the first kernel, the second sediment of external sheath Silicon dioxide, hydrate；

S30: stannic chloride pentahydrate and antimony trichloride are dissolved into containing acetylacetone,2,4-pentanedione for 5%~15% by antimony mole doping concentration In dehydrated alcohol, sufficiently reaction is stirred, forms third solution, then distilled water, the steaming are slowly added dropwise into the third solution The volume ratio of distilled water dosage and the dehydrated alcohol dosage is that 1.4~1.8:100 displays aging after continuing stirring 1~2 hour Obtain Sb doped stannic hydroxide colloidal sol；

S31: the intermediate powder is added in the Sb doped stannic hydroxide colloidal sol simultaneously by the mass volume ratio of 2g/100ml Ultrasonic disperse is carried out, then sealing and standing, is formed using the intermediate powder as the second kernel, external sheath Sb doped hydroxide The third sediment of tin；

S35: it dries, answering of calcining that the third sediment obtains that nano antimony-doped tin dioxide coats that second kernel formed Synkaryon shell structural nano powder；

S40: 4~9 parts of water soluble acrylic acids are added using 1 part of compound nuclear shell structure nano powder as additive by mass fraction In coating；

S45: ultrasonic disperse is dispersed in the compound nuclear shell structure nano powder in the water-borne acrylic coatings, shape At nanometer heat isolation paint.

2. a kind of nanometer heat isolation paint preparation method according to claim 1, it is characterised in that: in step slo, described The molar concentration of hydrochloric acid solution is 1~3mol/L.

3. a kind of nanometer heat isolation paint preparation method according to claim 1, it is characterised in that: described super in step S31 Sound jitter time is 15~30 minutes, and the sealing and standing time is 16~32 hours.

4. a kind of nanometer heat isolation paint preparation method according to claim 1, it is characterised in that: in step S15, S25 and In S35, the temperature of the calcining is 500~800 DEG C, and calcination time is 1~3 hour.

5. a kind of nanometer heat isolation paint preparation method described according to claim 1~any one of 4, it is characterised in that: Between step S11 and S15, further include the steps that first sediment is filtered, washed and dried before calcination.

6. a kind of nanometer heat isolation paint preparation method according to claim 5, it is characterised in that: step S21 and S25 it Between, further include the steps that second sediment is filtered, washed and dried before calcination.

7. a kind of nanometer heat isolation paint preparation method according to claim 5, it is characterised in that: step S31 and S35 it Between, further include the steps that the third sediment is filtered, washed and dried before calcination.

8. a kind of nanometer heat isolation paint preparation method according to claim 5, it is characterised in that: in step S40, the water Property acrylic coating by mass fraction by 40~70 parts of aqueous acrylic emulsions, 5~10 parts of calcium carbonate, 5~10 parts of mica powders, 1 ~5 parts of defoaming agents, 1~5 part of thickener and 1~20 part of water composition.

9. a kind of nanometer heat isolation paint preparation method according to claim 5, it is characterised in that: described super in step S45 The time of sound dispersion is 15~30 minutes.