CN114958065A - High-reflection heat-insulation type functional filler and preparation method and application thereof - Google Patents
High-reflection heat-insulation type functional filler and preparation method and application thereof Download PDFInfo
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
The invention discloses a high-reflection heat-insulation type functional filler and a preparation method and application thereof; firstly, dispersing potassium titanate whiskers in a strong alkali aqueous solution, stirring at room temperature for etching, and performing suction filtration, washing and drying to obtain pretreated potassium titanate whiskers; dissolving zinc salt in an organic solvent to obtain a solution A; dissolving the pretreated potassium titanate whiskers in deionized water, and treating the solution by using a cell crusher to obtain a solution B; adding the solution B into the solution A, adding a NaOH aqueous solution, and uniformly stirring to obtain a solution C; cooling the solution C to room temperature, adding ammonium salt, stirring at constant temperature, filtering, washing, drying and calcining to obtain the high-reflection heat-insulation functional filler, wherein the filler shows higher reflectivity at each wavelength; when the addition amount of the filler in the coating reaches 10%, the heat insulation temperature difference can reach 14.9 ℃, and the coating has an excellent heat insulation effect and can be applied to the fields of buildings, military affairs, national defense, aerospace and the like.
Description
Technical Field
The invention relates to a heat-insulating reflective filler, in particular to a preparation method and application of a high-reflection heat-insulating functional filler, belonging to the technical field of heat-insulating coatings.
Background
Since the 70 s of the 20 th century, with the rapid development of global economy, various energy consumptions are enormous, and mankind faces an unprecedented energy crisis. Energy sourceThe crisis is not only a problem faced by a certain country, but also a great burden that all mankind should share, and to solve the energy crisis, not only new energy needs to be searched from the source, but also energy needs to be saved, and long-term and sustainable development of energy is realized. The earth needs energy from the sun, such as wind energy, water energy, chemical energy, etc., which are directly or indirectly converted from solar energy. Today solar energy can still be 1.765 x 10 17 The speed of J/s is irradiated to the earth surface, the temperature of the object on the earth surface is continuously raised in summer under the continuous irradiation of sunlight, the temperature of the building roof can reach 40-50 ℃, and the temperature of the metal surface can reach 80-90 ℃. The gathering and dispersion of energy brings great inconvenience to the life of people. Building energy consumption has an important proportion among various energy consumption types and will show a trend of rising year by year in the future. In hot summer, the annual power consumption of refrigerating devices such as air conditioners, electric fans and the like accounts for 27 percent of the annual energy consumption of China. In winter with severe cold in the north, people need a large number of heating devices to keep out the cold, and the energy consumption of the cold-keeping devices accounts for 30% -50% of the energy consumption of buildings. The use of equipment for warming in winter and cooling in summer causes serious energy waste, so that the improvement of the heat preservation effect in winter and the heat insulation effect in summer of the building is of great significance. For the countries with large energy consumption, especially the countries with high building energy consumption, it is necessary to adopt the measures of reflecting sunlight and insulating heat for buildings.
Besides in the field of construction, reflective thermal insulation coatings are also applied in the field of national defense and military products: when the advanced high-tech products such as some military equipment, aircrafts, instruments and equipment are used, if the surface temperature is too high, the normal work of the products can be influenced, and the external heat can be blocked and reflected by coating the reflective heat-insulating coating on the outer surface of the products, so that the temperature of the surface and the inside of the equipment is reduced, and the problems are solved. However, most of the currently used military coating raw materials contain high-toxicity solvents, so that the environment is polluted, the safety coefficient is low, the mechanical and physical properties are low, the environmental protection effect is poor, and the coating is degraded after being irradiated by sunlight for a long time, so that the weather resistance and the durability of the coating are poor.
The Chinese patent application CN 104293012A discloses a heat-reflecting heat-insulating coating and a preparation method thereof, the method firstly pretreats hollow fibers to improve the reflection performance and the heat-insulating performance of the hollow fibers, then introduces modified polyvinylidene fluoride resin to increase the heat-resistant performance of the coating, and finally mixes fluorocarbon resin, polyvinylidene fluoride resin, epoxy resin, polyacrylamide, the hollow fibers, titanium dioxide and silicon dioxide according to a certain proportion to prepare the heat-reflecting heat-insulating coating. The method has the advantages that the prepared heat reflection heat insulation coating has good reflection heat insulation performance; the disadvantages are that the addition amount of the functional filler is high in the preparation process, the film forming state of the coating is influenced in practical application, and the cost is too high.
The Chinese patent application CN102558912A discloses a preparation method of a reflective functional filler, which is to coat a mixed solution of tin and antimony chlorides on the surface of hollow glass beads by utilizing ultrasonic atomization to prepare the reflective functional filler. The method has the advantages that the hollow glass beads with the heat preservation and insulation effects are compounded with the tin antimony oxide semiconductor heat reflection material, and the prepared filler has the advantages of the hollow glass beads and the tin antimony oxide semiconductor heat reflection material; however, antimony tin oxide shows reflection characteristics only in the near-mid infrared region, and has insufficient reflection effect on light in other bands, thereby greatly limiting the application range of the filler.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provide a high-reflection heat-insulation functional filler which has the advantages of cheap and easily-obtained raw materials, simple process, low cost, excellent reflection performance in visible light and infrared light regions and capability of realizing the target of reflection heat insulation by only adding a small amount of the filler in industrial production and a preparation method thereof.
The invention also aims to provide the application of the high-reflection heat-insulation functional filler in the preparation of the high-reflection heat-insulation coating, wherein when the content of the high-reflection heat-insulation functional filler in the high-reflection heat-insulation coating is 1%, 5% and 10%, the heat insulation temperature difference sequentially reaches 5.1 ℃, 11.1 ℃ and 15 ℃, and the high-reflection heat-insulation coating has an excellent heat insulation effect.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-reflection heat-insulation type functional filler comprises the following steps:
1) dispersing the potassium titanate whiskers in a strong alkali aqueous solution, stirring at room temperature for etching, and performing suction filtration, washing and drying to obtain pretreated potassium titanate whiskers;
2) dissolving zinc salt in an organic solvent to obtain a solution A; dissolving the pretreated potassium titanate whiskers in deionized water, and treating the solution by using a cell crusher to obtain a solution B;
3) adding the solution B into the solution A, adding NaOH aqueous solution, and uniformly stirring at the temperature of 50-90 ℃ to obtain solution C; the molar ratio of potassium titanate to zinc is 1: 0.1-1: 2;
4) and cooling the solution C to room temperature, adding ammonium salt, stirring at constant temperature, filtering, washing, drying and calcining to obtain the high-reflection heat-insulation functional filler (PTW @ ZnO).
In order to further achieve the purpose of the invention, preferably, the strong base is one or more of sodium hydroxide, potassium hydroxide and barium hydroxide, the concentration of the strong base aqueous solution is 5 wt% to 20 wt%, and the concentration of the potassium titanate whisker in the strong base aqueous solution is 0.05g/L to 0.1 g/L.
Preferably, the time for etching by stirring at room temperature is 12-24 h.
Preferably, the zinc salt is one or more of zinc sulfate, zinc acetate, zinc nitrate and basic zinc carbonate; zn in the solution A 2+ The concentration of (B) is 0.005mol/L to 0.05 mol/L.
Preferably, the organic solvent is one or more of ethanol, diethyl ether, dimethyl sulfoxide, isopropanol and tetrahydrofuran; the concentration of the potassium titanate whisker in the solution B is 0.02 mol/L-0.08 mol/L.
Preferably, the stirring time at the temperature of between 50 and 90 ℃ is between 20 and 60 min.
Preferably, the concentration of the added NaOH aqueous solution is 0.1-2 mol/L; the mass of the added ammonium salt is 0.05 g-5 g, and the stirring temperature is 50-90 ℃ at constant temperature.
Preferably, the calcining temperature is 300-600 ℃, and the calcining time is 0.5-2 h.
A high-reflection heat-insulation type functional filler is prepared by the preparation method.
The application of the high-reflection heat-insulation functional filler in preparing the high-reflection heat-insulation coating is as follows: according to the mass parts, 75-90 parts of water-based silicone-acrylic emulsion, 1-10 parts of high-reflection heat-insulation type functional filler, 5.0-8.0 parts of dodecyl alcohol ester film-forming aid, 0.01-0.03 part of defoaming agent and 0.03-0.05 part of pH regulator are uniformly mixed at room temperature for 0.5-2 hours to prepare the high-reflection heat-insulation coating.
The invention relates to a preparation method and application of a high-reflection heat-insulation functional filler, which comprises the steps of firstly mixing potassium titanate whiskers and zinc salts at a certain temperature, introducing an alkaline condition to hydrolyze the zinc salts into zinc hydroxide to coat the zinc hydroxide on the surfaces of the potassium titanate whiskers, wherein the addition of ammonium salt can consume hydroxide radicals in a solution to promote a hydrolysis reaction, successfully removing an organic solvent on the surfaces of the fillers after suction filtration and washing for several times, and dehydrating the zinc hydroxide to generate zinc oxide particles through high-temperature calcination to finally obtain the zinc oxide-coated potassium titanate whiskers. The stirring speed and temperature during the reaction are used for adjusting the size of zinc oxide particles, and the reaction time is used for controlling the coating rate of zinc oxide. The raw materials are cheap and easy to obtain, the process is simple, the cost is low, the heat insulation filler with high reflectivity can be obtained only through the normal pressure step, and the coating with the reflection heat insulation effect can be obtained after the heat insulation filler is mixed with the emulsion.
Compared with the reflective filler in the prior art, the invention has the following beneficial effects:
1. the potassium titanate whisker and the zinc oxide both have high refractive indexes, and the high-reflection heat-insulation type functional filler prepared by compounding the potassium titanate whisker and the zinc oxide has obvious advantages in refractive index, and particularly can realize the aim of reflection heat insulation by adding a small amount in industrial production: the reflectivity in visible light and infrared light areas is larger than 90%, and when the addition amounts are 1%, 5% and 10%, the heat insulation temperature difference respectively reaches 5.1 ℃, 11.1 ℃ and 15 ℃, so that the application cost is greatly saved.
2. Before coating, the surface of the potassium titanate whisker is pretreated to roughen the surface, and the rough surface provides a plurality of crystal nucleus growth sites, so that zinc oxide directly grows on the surface of the potassium titanate whisker, and the coating rate is improved. As can be seen from the comparison effect between fig. 1 and fig. 2 of the examples, the surface of the pretreated potassium titanate whisker is coated with a large amount of ZnO, and the coating amount is significantly improved compared with the non-pretreated potassium titanate whisker.
3. According to the invention, zinc oxide particles are coated on the surface of the potassium titanate whisker by adopting a heterogeneous precipitation method, and the potassium titanate whisker is used as a nucleation matrix.
4. The zinc oxide coated on the surface of the high-reflection heat-insulation type functional filler prepared by the invention is in a nanometer level, has a high specific surface area, enhances the reflection of light on the surface of the filler, and simultaneously can shield ultraviolet rays, so that the high-reflection heat-insulation type functional filler has certain application potential in the aspect of optics.
Drawings
FIG. 1 is a SEM image of ZnO coating before pretreatment obtained in example 1 of the present invention.
FIG. 2 is a SEM image of the pretreated ZnO coating obtained in example 1 of the present invention.
Fig. 3 is a comparative graph of the thermal insulation performance test obtained in example 4 of the present invention.
FIG. 4 is a comparison graph showing the diffuse reflectance test of the highly reflective heat insulating functional filler powder obtained in example 1 of the present invention and a commercially available reflective filler powder.
Detailed Description
For better understanding of the present invention, the present invention is further illustrated by the following examples, which are not intended to limit the scope of the claims of the present invention, and other examples obtained by those skilled in the art without inventive efforts shall fall within the scope of the present invention.
Example 1: synthesis of high-reflection heat-insulation type functional filler
0.75gK 2 Ti 6 O 13 Dispersing in 20g of 10 wt% NaOH aqueous solution, stirring at room temperature for 12h for etching, filtering, washing, and drying to obtain pretreated K 2 Ti 6 O 13 . 0.05g of Zn (Ac) 2 ·2H 2 O in 40ml of tetrahydrofuran, while 0.25g of pretreated K 2 Ti 6 O 13 The cells were pulverized by adding 10g of deionized water. Mixing the two solutions, heating to 55 deg.C, stirring at 500rpm for 30min, adding 0.8mol/L NaOH aqueous solution, cooling to room temperature, adding 0.1g NH 4 And Cl, stirring at the constant temperature of 55 ℃, and performing suction filtration, washing and drying to obtain the filler precursor. Calcining the precursor at 400 ℃ for 0.5h to obtain the potassium titanate whisker (PTW @ ZnO) coated by zinc oxide
FIG. 1 is a SEM image of ZnO coating before pretreatment obtained in example 1 of the present invention, in which fibrous substances are potassium titanate whiskers, and particulate substances having a particle size of about 300nm to 500nm are zinc oxide particles. As can be seen from this figure, the potassium titanate whisker surface is coated with a small amount of zinc oxide particles with non-uniform particle size.
FIG. 2 is a SEM image of the ZnO coating after pretreatment obtained in example 1 of the present invention, in which the fibrous substance is potassium titanate whisker and the particulate substance having a particle size of about 300nm to 500nm is zinc oxide particle. As can be seen from the figure, the surface of the potassium titanate whisker is coated by a large amount of zinc oxide particles with uniform particle size, and the coating amount is greatly improved compared with the SEM image without pretreatment.
FIG. 3 shows the results of a diffuse reflectance test of PTW @ ZnO and a commercially available reflective filler obtained in example 1 of the present invention, using a Perkinelmer LAMBDA 950 UV-visible near-IR spectrophotometer, to determine the diffuse reflectance of the paint film. As can be seen from FIG. 3, the reflectance of PTW @ ZnO in the wavelength range of 200nm to 2500nm is higher than that of the commercially available reflective fillers, that is, better reflection can be obtained by adding PTW @ ZnO to the emulsion.
Example 2: synthesis of high-reflection heat-insulation type functional filler
0.5gK 2 Ti 6 O 13 Dispersing in 15g of 15 wt% KOH aqueous solution, and stirring at room temperature for 20h for etchingEtching, filtering, washing and drying to obtain pretreated K 2 Ti 6 O 13 . 0.11g of ZnSO 4 Dissolved in 40ml of dimethyl sulfoxide, while 0.5g of pretreated K is added 2 Ti 6 O 13 15g of deionized water was added to the mixture to pulverize the cells. Mixing the two solutions, heating to 70 deg.C, stirring at 500rpm for 40min, adding 1.2mol/L NaOH aqueous solution, cooling to room temperature, and adding 1.8g NH 4 SO 4 Stirring at a constant temperature of 70 ℃, and performing suction filtration, washing and drying to obtain the filler precursor. Calcining the obtained precursor at 450 ℃ for 1h to obtain the potassium titanate whisker (PTW @ ZnO) coated by the zinc oxide.
And measuring the diffuse reflection data of the filler at 200 nm-2500 nm by using a Perkinelmer LAMBDA 950 ultraviolet visible near infrared spectrophotometer.
Example 3: synthesis of high-reflection heat-insulation type functional filler
1gK is added 2 Ti 6 O 13 Dispersed in 27g of 20 wt% Ba (OH) 2 Stirring in water solution at room temperature for 24h for etching, filtering, washing, and drying to obtain pretreated K 2 Ti 6 O 13 . 0.22g of Zn (NO) 3 ) 2 Dissolved in 40ml of ethanol while 0.1g of pretreated K is added 2 Ti 6 O 13 The cells were pulverized by adding 8g of deionized water. Mixing the two solutions, heating to 90 deg.C, stirring at 500rpm for 20min, adding 2mol/L NaOH aqueous solution, cooling to room temperature, and adding 4gNH 4 NO 3 Stirring at a constant temperature of 90 ℃, and performing suction filtration, washing and drying to obtain the filler precursor. Calcining the obtained precursor at 600 ℃ for 2h to obtain the potassium titanate whisker (PTW @ ZnO) coated by the zinc oxide.
Potassium titanate whiskers (PTW @ ZnO) coated with zinc oxide as a high-reflection heat-insulation functional filler with good dispersibility can be prepared by the above-mentioned examples 1 to 3. The potassium titanate whisker applied by the invention has high reflectivity due to the unique triangular prism appearance, and in addition, the characteristic that the thermal conductivity of the potassium titanate whisker is reduced along with the rise of temperature plays an important role in heat insulation. In addition, the potassium titanate whisker and the zinc oxide both have high refractive indexes, the high-reflection heat insulation type functional filler prepared by compounding the potassium titanate whisker and the zinc oxide has a refractive index value superior to that of the former two fillers, the target of reflection heat insulation can be realized by only adding a single and a small amount of filler in industrial production, the reflectivity in visible light and infrared light areas is more than 90%, and when the addition amounts are 1%, 5% and 10%, the heat insulation temperature difference respectively reaches 5.1 ℃, 11.1 ℃ and 15 ℃, so that the cost is greatly saved.
The surface of the potassium titanate whisker is pretreated before preparation, so that the surface of the potassium titanate whisker becomes rough, and the rough surface provides a plurality of crystal nucleus growth sites, thereby being beneficial to the direct growth of zinc oxide on the surface and improving the coating rate. The invention adopts a homogeneous precipitation method to coat zinc oxide particles on the surface of the potassium titanate whisker, takes the potassium titanate whisker as a nucleation substrate, and has simple process flow and uniform coating. In the invention, ammonium salt is added in the process of preparing the high-reflection heat-insulation type functional filler to promote the hydrolysis of zinc salt, and according to a chemical equation:
NH 4+ +OH - ＝NH 3 ·H 2 o, the existence of ammonium salt can greatly improve the hydrolysis efficiency of the zinc salt. The finally prepared high-reflection heat-insulation type functional filler has good dispersibility, and a dispersing agent is not required to be added during dispersion, so that the industrial application is facilitated.
Example 4: application of high-reflection heat-insulation type functional filler
Mixing and stirring the potassium titanate whisker (PTW @ ZnO) coated with the zinc oxide obtained in the example 1, the water-based silicone-acrylic emulsion, the functional additive and the deionized water; according to the mass percentage, the PTW @ ZnO water dispersion containing 1 wt% of solid accounts for 5%, the water-based silicone-acrylic emulsion accounts for 85%, the film-forming aid dodecyl alcohol ester accounts for 5%, the defoaming agent accounts for 0.01%, the flatting agent accounts for 0.1%, the pH regulator accounts for 0.03%, 8.86% of deionized water is added, and then the mixture is magnetically stirred for 0.5 hour to be uniformly dispersed. And finally, respectively scrubbing the aluminum plate by using 10 wt% of sodium hydroxide and 10 wt% of sulfuric acid in sequence, washing the aluminum plate by using deionized water for 2 times, and drying the aluminum plate for later use. The prepared high-reflection heat insulation coating and the water-based silicone-acrylic emulsion without filler are respectively coated on 1060 aluminum plates with the thickness of 100mm multiplied by 50mm multiplied by 1mm by using surfaces with different thicknesses of a BGD four-side preparation device to prepare samples with the coating thickness of 150um, and the samples are subjected to film forming in an electrothermal blowing constant-temperature drying oven at the temperature of 80 ℃ for 3 days for testing.
Example 5: application of high-reflection heat-insulation type functional filler
The PTW @ ZnO, the water-based silicone-acrylate emulsion, the functional additive and the deionized water obtained in the example 1 are mixed and stirred, according to the mass percentage, the PTW @ ZnO water dispersion containing 5 wt% of solid content, the water-based silicone-acrylate emulsion containing 75 wt% of solid content, the film forming additive dodecyl alcohol ester containing 5 wt% of film forming additive, the defoaming agent containing 0.01 wt% of film forming additive, the leveling agent containing 0.1 wt% of film forming additive and the pH regulator containing 0.03 wt% of film forming additive, 14.86% of deionized water is added, and then the mixture is magnetically stirred for 1 hour to be uniformly dispersed. Finally, respectively scrubbing the aluminum plate by using 10 wt% sodium hydroxide and 10 wt% sulfuric acid, washing the aluminum plate by using deionized water for 2 times, and drying the aluminum plate for later use. The prepared high-reflection heat insulation coating and the water-based silicone-acrylic emulsion without filler are respectively coated on 1060 aluminum plates with the thickness of 100mm multiplied by 50mm multiplied by 1mm by using surfaces with different thicknesses of a BGD four-side preparation device to prepare samples with the coating thickness of 150um, and the samples are subjected to film forming in an electrothermal blowing constant-temperature drying oven at the temperature of 80 ℃ for 3 days for testing.
Example 6: application of high-reflection heat-insulation type functional filler
The PTW @ ZnO, the water-based silicone-acrylate emulsion, the functional additive and the deionized water obtained in the example 1 are mixed and stirred, according to the mass percentage, the PTW @ ZnO water dispersion containing 10 wt% of solid accounts for 5%, the water-based silicone-acrylate emulsion accounts for 75%, the film forming additive dodecyl alcohol ester accounts for 5%, the defoaming agent accounts for 0.01%, the flatting agent accounts for 0.1%, the pH regulator accounts for 0.03%, 9.86% of deionized water is added, and then the mixture is stirred magnetically for 0.5 hour to be uniformly dispersed. Finally, respectively scrubbing the aluminum plate by using 10 wt% sodium hydroxide and 10 wt% sulfuric acid, washing the aluminum plate by using deionized water for 2 times, and drying the aluminum plate for later use. The prepared high-reflection heat insulation coating and the water-based silicone-acrylic emulsion without filler are respectively coated on 1060 aluminum plates with the thickness of 100mm multiplied by 50mm multiplied by 1mm by using surfaces with different thicknesses of a BGD four-surface preparation device to prepare a sample with the coating film thickness of 150 mu m, and the sample is subjected to film forming in an electric heating air blowing constant-temperature drying box at the temperature of 80 ℃ for 3 days for testing.
The paint film properties were tested according to the standard for examples 4 to 6:
and (3) building a heat insulation device according to the standard specified in JGT235-2008 reflective heat insulation coating for buildings, and testing the heat insulation temperature difference of the heat insulation coating.
The hardness of the coating was tested according to the national standard GB/T6739-1996.
The adhesion of the coating was tested by the cross-hatch method, according to the specifications of the national standard GB/T9286-1998.
The water resistance of the coating was tested as specified in the national Standard GB/T1733-1993A method.
The acid resistance of the coating was tested as specified in the national standard GB/T9274-1988A.
The coatings were tested for alkali resistance as specified in the national standard GB/T9274-1998A.
FIG. 3 is a graph showing a comparison of the insulation temperature difference obtained in examples 4 to 6 of the present invention: the heat insulation device is built according to the standard specified in JGT235-2008 reflective heat insulation coating for buildings, the heating lamp starts to work, the timing is stopped when the test temperature is gentle, the temperature difference between the sample and the blank group is the heat insulation temperature difference, and the larger the heat insulation temperature difference value is, the more remarkable the heat insulation effect of the coating is. The figure shows that the high-reflection heat insulation type functional filler in the high-reflection heat insulation coating has the heat insulation temperature difference of 5.1 ℃, 11.1 ℃ and 15 ℃ when the content is 1%, 5% and 10%, has excellent heat insulation effect, and can be applied to the field of buildings, military affairs, national defense, aerospace and other advanced high-tech fields. In practical application, zinc oxide coated potassium titanate whiskers (PTW @ ZnO) with different contents can be added according to the heat insulation requirement of the actual situation so as to meet the requirement.
The results of the other experiments are shown in table 1 below.
TABLE 1
It can be seen from table 1 that with the addition of the nano filler, the pencil hardness of the paint film of the high-reflection heat insulation coating reaches 4H at most, and the adhesive force also reaches 0 level, which indicates that the coating has excellent friction resistance and impact resistance, because the zinc oxide is used as the metal oxide to improve the hardness of the coating, and the rough surface of the potassium titanate whisker (PTW @ ZnO) coated by the zinc oxide enhances the adhesion between the coating and the base material. Compared with a pure silicon acrylic paint film without filler, the comprehensive performance is comprehensively improved, and various weather resistance tests pass the tests, so that the existing heat-insulating paint is achieved. The test results of the highly reflective thermal insulating functional filler of examples 2 and 3 are similar to those of the present example and are not provided.
Comparative example
The reflective heat-insulating filler ceramic micro powder (HG-T600) of Shanghai Huizi sub-nanometer new material company Limited is adopted to replace PTW @ ZnO in the embodiment 4, the reflective coating is prepared and coated by the same steps, and the test is carried out:
the paint film properties were tested according to the standard:
and (3) building a heat insulation device according to the standard specified in JGT235-2008 reflective heat insulation coating for buildings, and testing the highest heat insulation temperature difference of the heat insulation coating.
The hardness of the coating was tested according to the national standard GB/T6739-1996.
The adhesion of the coating was tested by the cross-hatch method, according to the specifications of the national standard GB/T9286-1998.
The diffuse reflectance data of PTW @ ZnO and commercially available reflective fillers at 200nm to 2500nm was measured using a Perkinelmer LAMBDA 950 ultraviolet visible near infrared spectrophotometer. FIG. 4 is a comparison graph of the PTW @ ZnO and a commercially available reflective filler powder in a diffuse reflection test, and it can be seen from the graph that the reflectivity of the PTW @ ZnO in a wavelength range of 200-2500 nm is better than that of a reflective heat-insulating filler ceramic micropowder (HG-T600).
The test results of inventive example 6 and comparative example are shown in table 2 below.
TABLE 2
The table 2 shows that the heat insulation temperature difference of the high-reflection heat insulation coating is 11.3 ℃ higher than that of the reflection coating, the pencil hardness and the adhesive force performance of the high-reflection heat insulation coating are both superior to those of the reflection coating prepared by the reflection filler sold in the market, and the comprehensive performance of the high-reflection heat insulation coating is excellent.
Under the premise of realizing the thermal insulation temperature difference of 15 ℃, the addition amount of the functional filler in the Chinese patent application CN 104293012A reaches 25% of that of the film forming substance, while the addition amount of the zinc oxide coated potassium titanate whisker (PTW @ ZnO) prepared in the invention only needs 10% of that of the film forming substance, which shows that the high-reflection thermal insulation type functional filler has more excellent thermal insulation effect, and probably the potassium titanate whisker used in the invention has the characteristic that the thermal conductivity is reduced along with the temperature rise. The filler prepared in the Chinese patent application CN102558912A shows excellent reflection characteristics only in near and middle infrared regions, while the zinc oxide coated potassium titanate whisker (PTW @ ZnO) prepared by the invention shows excellent reflection performance in visible light and infrared light regions, probably because of the high reflection property of the potassium titanate whisker and the coordination effect after zinc oxide coating.
It should be noted that the present invention is not limited by the above-mentioned embodiments, and various changes and modifications can be made in the present invention without departing from the spirit and scope of the present invention, and these changes and modifications fall into the protection scope of the claimed invention; the scope of the invention is defined by the following claims.
Claims (10)
1. A preparation method of a high-reflection heat-insulation type functional filler is characterized by comprising the following steps:
1) dispersing potassium titanate whiskers in a strong alkaline aqueous solution, stirring at room temperature for etching, and performing suction filtration, washing and drying to obtain pretreated potassium titanate whiskers;
2) dissolving zinc salt in an organic solvent to obtain a solution A; dissolving the pretreated potassium titanate whiskers in deionized water, and treating the solution by using a cell crusher to obtain a solution B;
3) adding the solution B into the solution A, adding NaOH aqueous solution, and uniformly stirring at the temperature of 50-90 ℃ to obtain solution C; the molar ratio of potassium titanate to zinc is 1: 0.1-1: 2;
4) and cooling the solution C to room temperature, adding ammonium salt, and stirring at constant temperature, filtering, washing, drying and calcining to obtain the high-reflection heat-insulation functional filler.
2. The method for preparing the high-reflection heat insulation type functional filler according to claim 1, wherein the method comprises the following steps: the strong base is one or more of sodium hydroxide, potassium hydroxide and barium hydroxide, the concentration of the strong base aqueous solution is 5-20 wt%, and the concentration of the potassium titanate whisker in the strong base aqueous solution is 0.05-0.1 g/L.
3. The method for preparing the high-reflection heat insulation type functional filler according to claim 1, wherein the method comprises the following steps: the time for stirring at room temperature for etching is 12-24 h.
4. The method for preparing the high-reflection heat insulation type functional filler according to claim 1, wherein the method comprises the following steps: the zinc salt is one or more of zinc sulfate, zinc acetate, zinc nitrate and basic zinc carbonate; zn in the solution A 2+ The concentration of (B) is 0.005mol/L to 0.05 mol/L.
5. The method for preparing the high-reflection heat insulation type functional filler according to claim 1, wherein the method comprises the following steps: the organic solvent is one or more of ethanol, diethyl ether, dimethyl sulfoxide, isopropanol and tetrahydrofuran; the concentration of the potassium titanate whisker in the solution B is 0.02 mol/L-0.08 mol/L.
6. The preparation method of the high-reflectivity functional filler of claim 1, wherein the preparation method comprises the following steps: the stirring time at the temperature of 50-90 ℃ is 20-60 min.
7. The method for preparing the high-reflection heat insulation type functional filler according to claim 1, wherein the method comprises the following steps: the concentration of the added NaOH aqueous solution is 0.1-2 mol/L; the mass of the added ammonium salt is 0.05 g-5 g, and the stirring temperature is 50-90 ℃ at constant temperature.
8. The method for preparing the high-reflectivity heat-insulating functional filler according to claim 1, wherein the method comprises the following steps: the calcining temperature is 300-600 ℃, and the calcining time is 0.5-2 h.
9. A high-reflection heat-insulation type functional filler, which is prepared by the preparation method of any one of claims 1 to 8.
10. Use of the high reflective insulation type functional filler according to claim 9 for preparing a high reflective insulation coating; the method is characterized in that: according to the mass parts, 75-90 parts of water-based silicone-acrylic emulsion, 1-10 parts of high-reflection heat-insulation type functional filler, 5.0-8.0 parts of dodecyl alcohol ester film-forming aid, 0.01-0.03 part of defoaming agent and 0.03-0.05 part of pH regulator are uniformly mixed at room temperature for 0.5-2 hours to prepare the high-reflection heat-insulation coating.
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