A method for preparing aluminum phosphate material with high radiation performance in atmospheric window

Abstract

The present invention discloses a method for preparing an aluminum phosphate material with high radiation performance at an atmospheric window. A MOF precursor is prepared by a microwave ultrasonic ultraviolet reactor and a hydrothermal method, and finally aluminum phosphate with a monoclinic crystal form is synthesized at a certain calcination temperature. The prepared aluminum phosphate has excellent solar reflectivity and excellent mid-infrared emissivity, exhibits excellent performance in the field of radiation cooling, and also exhibits certain radiation cooling performance in ceramic coatings.

Description

Technical Field

[0001] The present invention relates to the technical field of radiation refrigeration materials, and in particular to a method for preparing an aluminum phosphate material with high radiation performance in an atmospheric window. Background Art

[0002] As the greenhouse effect intensifies and hotter weather continues to drive demand for cooling, active cooling methods, such as fans and air conditioners, consume significant amounts of electricity, and the power generation methods used only further contribute to the greenhouse effect. Radiative cooling is a new, clean, and efficient passive cooling method that achieves cooling without consuming additional energy. New and efficient radiative cooling materials have become a focus of research.

[0003] Currently, the main methods for developing radiative cooling materials include hydrothermal, solvothermal, template, and co-precipitation. While these methods can yield high-purity and controlled morphology, they all require complex and sophisticated equipment, take a long time to synthesize, and have low yields, making them unsuitable for mass production. Summary of the Invention

[0004] In view of the shortcomings of the existing technology, the purpose of the present invention is to provide a method for preparing an aluminum phosphate material with high radiation performance at the atmospheric window, which is prepared by preparing a MOF precursor through a microwave ultrasonic ultraviolet reactor and a hydrothermal method and finally synthesizing a monoclinic aluminum phosphate at a certain calcination temperature. The prepared aluminum phosphate has excellent solar reflectivity and excellent mid-infrared emissivity, exhibits excellent performance in the field of radiation refrigeration, and also exhibits certain radiation refrigeration performance in ceramic coatings.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is as follows: a method for preparing an aluminum phosphate material with high radiation performance in an atmospheric window, comprising the following steps:

[0006] (1) preparing a solution A containing 0.1 to 1 mol / L AlCl3·6H2O; adding terephthalic acid and 2-aminophthalic acid to N,N-dimethylacetamide, respectively, and stirring evenly to obtain a solution B containing 0.1 to 1 mol / L terephthalic acid and 2-aminophthalic acid;

[0007] The solution A is fully stirred with the solution B to obtain solution C, wherein Al 3+ The molar ratio of phthalic acid: 2-aminophthalic acid is (1-3): (1-3): (1-3);

[0008] (2) Prepare solution D with the contents of sodium dihydrogen phosphate and ammonium phosphate both ranging from 0.1 to 1 mol / L;

[0009] Add the D solution to the C solution, and stir the mixture at 50-90°C for 2-6 hours to obtain the F solution, wherein the sodium dihydrogen phosphate: ammonium phosphate: Al 3+ The molar ratio is (1-3): (1-3): (1-3);

[0010] (3) placing the F solution in a microwave ultrasonic ultraviolet reactor and irradiating it with ultraviolet light of 365 nm at a power of 300-600 W for 2-5 h, then transferring the reaction solution to a hydrothermal reactor, placing the hydrothermal reactor containing the reaction solution in an oven, reacting at 100-180° C. for 8-12 h, and cooling to room temperature to obtain a G solution;

[0011] (4) The G solution is evaporated by rotary evaporation to collect the product to obtain product H; the product H is placed in a vacuum drying oven at 70-200° C. for 2-5 hours to obtain product I;

[0012] (5) placing the product I in a muffle furnace, heating it to 280-320°C at a rate of 7-9°C / min, and keeping it warm for 28-32 minutes; then heating it to 700-1000°C at a rate of 9-11°C / min, and keeping it warm for 1-3 hours to obtain product J; the product J is an aluminum phosphate material with high radiation performance in the atmospheric window.

[0013] Furthermore, in step (1), the solution A is fully stirred with the solution B to obtain a solution C, wherein Al 3+ The molar ratio of phthalic acid:2-aminophthalic acid is (2-3):(2-3):(2-3).

[0014] Furthermore, in the step (2), the D solution is added to the C solution, and the mixture is stirred at 70-90°C for 4-6 hours to obtain the F solution, wherein the mixture is sodium dihydrogen phosphate: ammonium phosphate: Al 3+ The molar ratio is (2~3):(2~3):(2~3).

[0015] Furthermore, in the step (3), the F solution is placed in a microwave ultrasonic ultraviolet reactor and irradiated with ultraviolet light of a wavelength of 365 nm at a power of 300 to 600 W for 3 to 5 hours, and then the reaction liquid is transferred to a hydrothermal reactor, and the hydrothermal reactor containing the reaction liquid is placed in an oven, reacted at 130 to 180° C. for 10 to 12 hours, and cooled to room temperature to obtain a G solution.

[0016] Furthermore, in the step (4), the G solution is evaporated by a rotary evaporator to collect the product to obtain product H; the product H is placed in a vacuum drying oven and dried at 120-200° C. for 3-5 hours to obtain product I.

[0017] Furthermore, in the step (5), the product I is placed in a muffle furnace, heated to 300-320°C at a rate of 8-9°C / min, and kept warm for 30-32 minutes; then heated to 900-1000°C at a rate of 10-11°C / min, and kept warm for 2-3 hours to obtain product J; the product J is an aluminum phosphate material with high radiation performance in the atmospheric window.

[0018] Furthermore, the method for using the prepared aluminum phosphate material with high radiation performance in the atmospheric window is as follows: 1) weighing 2 to 5 parts by weight of washed kaolin, 30 to 40 parts by weight of frit, 1 to 4 parts by weight of sodium tripolyphosphate, 3 to 5 parts by weight of feldspar, and 1 to 4 parts by weight of the product J; putting them together in a ball mill and ball milling them, and passing the ball-milled slurry through a 200-mesh sieve to obtain a functional layer glaze; 2) applying the functional layer glaze to ultra-white green bricks, drying, and firing to obtain ceramic tiles covered with a functional coating.

[0019] Furthermore, the method for using the prepared aluminum phosphate material with high radiation performance in the atmospheric window is as follows: 1) weighing 3 to 5 parts by weight of washed kaolin, 35 to 40 parts by weight of frit, 3 to 4 parts by weight of sodium tripolyphosphate, 4 to 5 parts by weight of feldspar, and 3 to 4 parts by weight of the product J; putting them together in a ball mill and ball milling them, and passing the ball-milled slurry through a 200-mesh sieve to obtain a functional layer glaze; 2) applying the functional layer glaze to ultra-white green bricks, drying, and firing to obtain ceramic tiles covered with a functional coating.

[0020] Furthermore, in the step 2), the functional layer glaze is coated on the ultra-white blank brick, and placed in an oven for drying to obtain dried ultra-white blank brick; the dried ultra-white blank brick is placed in an electric furnace, heated to 800-1000°C at a heating rate of 7-10°C / min, and kept warm for 18-22 minutes to obtain ceramic tiles covered with a functional coating.

[0021] Furthermore, in the step 2), the functional layer glaze is coated on the ultra-white blank brick, and placed in an oven for drying to obtain dried ultra-white blank brick; the dried ultra-white blank brick is placed in an electric furnace, heated to 950-1000°C at a heating rate of 8-10°C / min, and kept warm for 20-22 minutes to obtain ceramic tiles covered with a functional coating.

[0022] The present invention provides a method for preparing an aluminum phosphate material having high radiation performance in an atmospheric window, which has the following beneficial effects:

[0023] 1. The present invention prepares a MOF precursor by a hydrothermal method and synthesizes a monoclinic aluminum phosphate material at a certain temperature, and its morphology and structure are controllable.

[0024] 2. The preparation process of the present invention is simple, the raw materials are common, the controllability is strong, and the output is large, which is easy to realize industrial production.

[0025] 3. The synthesized monoclinic aluminum phosphate powder has both high solar reflectivity and high and medium infrared emissivity; it can not only reflect the strong heat from the sun, but also radiate its own heat into outer space in the form of infrared rays.

[0026] 4. The application of the powder obtained in the present invention in ceramic glazes has shown an excellent cooling effect through actual temperature measurement tests.

[0027] The present invention provides a method for preparing an aluminum phosphate material with high radiation performance at an atmospheric window, and also provides one of the methods for using the aluminum phosphate material with high radiation performance at an atmospheric window, optimizes the composition ratio of the functional layer glaze, and can effectively exert the excellent performance of the aluminum phosphate material with high radiation performance at an atmospheric window; it also optimizes the preparation method of ceramic tiles with functional coatings, and further improves the various performances of the prepared ceramic tiles covered with functional coatings. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 The XRD pattern of the aluminum phosphate material with high radiation performance in the atmospheric window prepared by the present invention is as follows; Figure 1 It can be seen that the crystal form of the aluminum phosphate material is monoclinic;

[0029] Figure 2 This is a SEM image of the aluminum phosphate material with high radiation performance in the atmospheric window prepared by the present invention; Figure 2 It can be seen that the morphology of the aluminum phosphate material is in the form of layered flakes, and the size is about 1.2 μm;

[0030] Figure 3 The reflectivity spectrum of the aluminum phosphate material with high radiation performance in the atmospheric window prepared by the present invention; Figure 3 It can be seen that the aluminum phosphate material has a high reflectivity of about 98%;

[0031] Figure 4 This is the emissivity spectrum of the aluminum phosphate material with high radiation performance in the atmospheric window prepared by the present invention; Figure 4 It can be seen that the aluminum phosphate material has a high emissivity of about 90% in the range of 8 to 13 μm;

[0032] Figure 5This is a diagram showing the actual cooling effect of the aluminum phosphate material with high radiation performance at the atmospheric window prepared by the present invention; Figure 5 It can be seen that the maximum temperature drop of the aluminum phosphate material in the actual environment is about 5°C;

[0033] Figure 6 This is a diagram showing the cooling effect of the aluminum phosphate material with high radiation performance in the atmospheric window prepared by the present invention when used in glaze; Figure 6 It can be seen that the cooling effect of the glaze layer with aluminum phosphate material added is about 4°C higher than that of the glaze layer without aluminum phosphate material added. DETAILED DESCRIPTION

[0034] The following examples are further given to illustrate the present invention in detail. It should be understood that the following examples are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above content of the present invention all fall within the scope of protection of the present invention. The specific process parameters and the like in the following examples are only examples within a suitable range, that is, those skilled in the art can make selections within a suitable range through the description herein, and are not limited to the specific numerical values exemplified below.

[0035] Example 1

[0036] A preparation method of an aluminum phosphate material having high radiation performance at an atmospheric window comprises the following steps:

[0037] Step 1: Dissolve 2.4143 g of AlCl₃·6H₂O in 50 ml of deionized water to obtain Solution A. Separately weigh 1.66 g of terephthalic acid and 1.8 g of 2-aminophthalic acid in 50 ml of N,N-dimethylacetamide (DMA) and stir thoroughly to obtain Solution B. Add Solution A to Solution B and stir thoroughly for 0.5 h to obtain Solution C. The molar ratio of Al₃⁺:phthalic acid:2-aminophthalic acid is 1:1:1.

[0038] Step 2: Dissolve 1.56g of sodium dihydrogen phosphate and 1.49g of ammonium phosphate in 50ml of deionized water and stir thoroughly to obtain Solution D. Add Solution D to Solution C and stir at 70°C for 2 hours to obtain Solution F. The molar ratio of sodium dihydrogen phosphate:ammonium phosphate:Al3+ is 1:1:1.

[0039] Step 3: Place solution F in a microwave ultrasonic UV reactor and irradiate with ultraviolet light of a wavelength of 365 nm at a power of 300 W for 2 h, then transfer it to a hydrothermal reactor (100 ml polytetrafluoroethylene lining), place it in an oven at 120°C for 8 h, and cool it to room temperature to obtain solution G.

[0040] Step 4: Pass the G solution through a rotary evaporator to collect the product to obtain product H, and then place product H in a vacuum drying oven at 70°C for 2 hours to obtain product I.

[0041] Step 5: Place the crucible containing product I in a muffle furnace, heat it to 300°C at a rate of 8°C / min, keep it warm for 30 minutes, then heat it to 900°C at a rate of 10°C / min, keep it warm for 1 hour, and obtain product J.

[0042] Step 6: Weigh 2g of washed kaolin, 30g of frit, 1g of sodium tripolyphosphate, 3g of feldspar, and 1g of prepared product J respectively and put them into a ball mill, add 20ml of water, and ball mill for 20min. After passing the ball-milled slurry through a 200-mesh sieve, brush it on an ultra-white blank brick and put it into an oven for drying.

[0043] Step 7: The dried ultra-white green bricks are kept at 800° C. in an electric furnace at a heating rate of 8° C. / min for 18 minutes to obtain ceramic bricks covered with a functional coating.

[0044] Example 2

[0045] A preparation method of an aluminum phosphate material having high radiation performance at an atmospheric window comprises the following steps:

[0046] Step 1: Weigh 4.8g of AlCl3·6H2O and dissolve it in 60ml of deionized water to obtain solution A. Weigh 3.7g of terephthalic acid and 3.6g of 2-aminophthalic acid respectively, add them into 60ml of N,N-dimethylacetamide (DMA) and stir thoroughly to obtain solution B. Add solution A into solution B and stir thoroughly for 1h to obtain solution C. 3+ The molar ratio of phthalic acid:2-aminophthalic acid is 1:2:2.

[0047] Step 2: Weigh 3g of sodium dihydrogen phosphate and 3g of ammonium phosphate respectively and dissolve them in 60ml of deionized water, then stir thoroughly to obtain solution D. Add solution D to solution C and stir at 50℃ for 3h to obtain solution F. 3+ The molar ratio is 1:2:1.

[0048] Step 3: Place solution F in a microwave ultrasonic UV reactor and irradiate with ultraviolet light of a wavelength of 365 nm at a power of 400 W for 3 h, then transfer it to a hydrothermal reactor (100 ml polytetrafluoroethylene lining), place it in an oven at 150°C for 9 h, and cool it to room temperature to obtain solution G.

[0049] Step 4: Pass the G solution through a rotary evaporator to collect the product to obtain product H, and then place product H in a vacuum drying oven at 100°C for 3 hours to obtain product I.

[0050] Step 5: Place the crucible containing product I in a muffle furnace, heat it to 300°C at a rate of 8°C / min, keep it warm for 30 minutes, then heat it to 700°C at a rate of 10°C / min, keep it warm for 2 hours, and obtain product J.

[0051] Step 6: Weigh 3g of washed kaolin, 35g of frit, 3g of sodium tripolyphosphate, 4g of feldspar, and 2g of prepared product J respectively and put them into a ball mill, add 24ml of water, and ball mill for 25min. After passing the ball-milled slurry through a 200-mesh sieve, brush it on an ultra-white blank brick and put it into an oven for drying.

[0052] Step 7: The dried ultra-white green bricks are kept at 900° C. in an electric furnace at a heating rate of 9° C. / min for 20 min to obtain ceramic bricks covered with a functional coating.

[0053] Example 3

[0054] A preparation method of an aluminum phosphate material having high radiation performance at an atmospheric window comprises the following steps:

[0055] Step 1: Weigh 7.5g of AlCl3·6H2O and dissolve it in 70ml of deionized water to obtain solution A. Weigh 4.7g of terephthalic acid and 5.4g of 2-aminophthalic acid respectively, add them into 70ml of N,N-dimethylacetamide (DMA) and stir thoroughly to obtain solution B. Add solution A into solution B and stir thoroughly for 1.5h to obtain solution C. 3+ The molar ratio of phthalic acid:2-aminophthalic acid is 2:1:2.

[0056] Step 2: Weigh 6g of sodium dihydrogen phosphate and 4.6g of ammonium phosphate and dissolve them in 70ml of deionized water, stir thoroughly to obtain solution D. Add solution D to solution C, stir and react at 70℃ for 4h to obtain solution F. 3+ The molar ratio is 2:2:1.

[0057] Step 3: Place solution F in a microwave ultrasonic UV reactor and irradiate with ultraviolet light of a wavelength of 365 nm at a power of 500 W for 4 h, then transfer it to a hydrothermal reactor (100 ml polytetrafluoroethylene lining), place it in an oven at 100°C for 10 h, and cool it to room temperature to obtain solution G.

[0058] Step 4: Pass the G solution through a rotary evaporator to collect the product to obtain product H, and then place product H in a vacuum drying oven at 120°C for 4 hours to obtain product I.

[0059] Step 5: Place the crucible containing product I in a muffle furnace, heat it to 300°C at a rate of 8°C / min, keep it warm for 30 minutes, then heat it to 900°C at a rate of 10°C / min, keep it warm for 2 hours, and obtain product J.

[0060] Step 6: Weigh 4g of washed kaolin, 37g of frit, 4g of sodium tripolyphosphate, 4g of feldspar, and 3g of prepared product J respectively and put them into a ball mill, add 28ml of water, and ball mill for 30min. After passing the ball-milled slurry through a 200-mesh sieve, brush it on an ultra-white blank brick and put it into an oven for drying.

[0061] Step 7: The dried ultra-white green bricks are kept at 950° C. in an electric furnace at a heating rate of 9° C. / min for 20 min to obtain ceramic bricks covered with a functional coating.

[0062] Example 4

[0063] A preparation method of an aluminum phosphate material having high radiation performance at an atmospheric window comprises the following steps:

[0064] Step 1: Weigh 24.14g of AlCl3·6H2O and dissolve it in 100ml of deionized water to obtain solution A. Weigh 16.6g of terephthalic acid and 17.9g of 2-aminophthalic acid respectively, add them into 100ml of N,N-dimethylacetamide (DMA) and stir thoroughly to obtain solution B. Add solution A into solution B and stir thoroughly for 2h to obtain solution C. 3+ The molar ratio of phthalic acid:2-aminophthalic acid is 3:2:2.

[0065] Step 2: Weigh 15.6g of sodium dihydrogen phosphate and 14.9g of ammonium phosphate respectively and dissolve them in 100ml of deionized water, then stir thoroughly to obtain solution D. Add solution D to solution C and stir at 90℃ for 6h to obtain solution F. 3+ The molar ratio is 2:2:3.

[0066] Step 3: Place solution F in a microwave ultrasonic UV reactor and irradiate with ultraviolet light of a wavelength of 365 nm at a power of 600 W for 5 h, then transfer it to a hydrothermal reactor (100 ml polytetrafluoroethylene lining), place it in an oven at 180°C for 12 h, and cool it to room temperature to obtain solution G.

[0067] Step 4: Pass the G solution through a rotary evaporator to collect the product to obtain product H, and then place product H in a vacuum drying oven at 200°C for 5 hours to obtain product I.

[0068] Step 5: Place the crucible containing product I in a muffle furnace, heat it to 300°C at a rate of 8°C / min, keep it warm for 30 minutes, then heat it to 1000°C at a rate of 10°C / min, keep it warm for 1 to 3 hours, and obtain product J.

[0069] Step 6: Weigh 5g of washed kaolin, 40g of frit, 1g of sodium tripolyphosphate, 5g of feldspar, and 4g of prepared product J respectively and put them into a ball mill, add 30ml of water, and ball mill for 60min. After passing the ball-milled slurry through a 200-mesh sieve, brush it on ultra-white blank bricks and put it into an oven for drying.

[0070] Step 7: The dried ultra-white green bricks are kept at 1000° C. in an electric furnace at a heating rate of 10° C. / min for 22 minutes to obtain ceramic bricks covered with a functional coating.

[0071] Example 5

[0072] A preparation method of an aluminum phosphate material having high radiation performance at an atmospheric window comprises the following steps:

[0073] Step 1: Weigh 7.5g of AlCl3·6H2O and dissolve it in 70ml of deionized water to obtain solution A. Weigh 4.7g of terephthalic acid and 5.4g of 2-aminophthalic acid respectively, add them into 70ml of N,N-dimethylacetamide (DMA) and stir thoroughly to obtain solution B. Add solution A into solution B and stir thoroughly for 1.5h to obtain solution C. 3+ The molar ratio of phthalic acid:2-aminophthalic acid is 2:1:2.

[0074] Step 2: Weigh 6g of sodium dihydrogen phosphate and 4.6g of ammonium phosphate and dissolve them in 70ml of deionized water, stir thoroughly to obtain solution D. Add solution D to solution C, stir and react at 70℃ for 4h to obtain solution F. 3+ The molar ratio is 2:2:1.

[0075] Step 3: Place solution F in a microwave ultrasonic UV reactor and irradiate with ultraviolet light of a wavelength of 365 nm at a power of 500 W for 4 h, then transfer it to a hydrothermal reactor (100 ml polytetrafluoroethylene lining), place it in an oven at 100°C for 10 h, and cool it to room temperature to obtain solution G.

[0076] Step 4: Pass the G solution through a rotary evaporator to collect the product to obtain product H, and then place product H in a vacuum drying oven at 120°C for 4 hours to obtain product I.

[0077] Step 5: Place the crucible containing product I in a muffle furnace, heat it to 300°C at a rate of 8°C / min, keep it warm for 30 minutes, then heat it to 900°C at a rate of 10°C / min, keep it warm for 2 hours, and obtain product J.

[0078] Step 6: Weigh 4g of washed kaolin, 37g of frit, 4g of feldspar, and 3g of prepared product J respectively and put them into a ball mill, add 28ml of water, and ball mill for 30min. After passing the ball-milled slurry through a 200-mesh sieve, brush it on an ultra-white blank brick and put it into an oven for drying.

[0079] Step 7: The dried ultra-white green bricks are kept at 950° C. in an electric furnace at a heating rate of 5° C. / min for 20 min to obtain ceramic bricks covered with a functional coating.

[0080] Example 6

[0081] A preparation method of an aluminum phosphate material having high radiation performance at an atmospheric window comprises the following steps:

[0082] Step 1: Weigh 7.5g of AlCl3·6H2O and dissolve it in 70ml of deionized water to obtain solution A. Weigh 4.7g of terephthalic acid and 5.4g of 2-aminophthalic acid respectively, add them into 70ml of N,N-dimethylacetamide (DMA) and stir thoroughly to obtain solution B. Add solution A into solution B and stir thoroughly for 1.5h to obtain solution C. 3+ The molar ratio of phthalic acid:2-aminophthalic acid is 2:1:2.

[0083] Step 2: Weigh 6g of sodium dihydrogen phosphate and 4.6g of ammonium phosphate and dissolve them in 70ml of deionized water, stir thoroughly to obtain solution D. Add solution D to solution C, stir and react at 70℃ for 4h to obtain solution F. 3+ The molar ratio is 2:2:1.

[0084] Step 3: Place solution F in a microwave ultrasonic UV reactor and irradiate with ultraviolet light of a wavelength of 365 nm at a power of 500 W for 4 h, then transfer it to a hydrothermal reactor (100 ml polytetrafluoroethylene lining), place it in an oven at 100°C for 10 h, and cool it to room temperature to obtain solution G.

[0085] Step 4: Pass the G solution through a rotary evaporator to collect the product to obtain product H, and then place product H in a vacuum drying oven at 120°C for 4 hours to obtain product I.

[0086] Step 5: Place the crucible containing product I in a muffle furnace, heat it to 300°C at a rate of 8°C / min, keep it warm for 30 minutes, then heat it to 900°C at a rate of 10°C / min, keep it warm for 2 hours, and obtain product J.

[0087] Step 6: Weigh 4g of washed kaolin, 37g of frit, 4g of feldspar, and 3g of prepared product J respectively and put them into a ball mill, add 28ml of water, and ball mill for 30min. After passing the ball-milled slurry through a 200-mesh sieve, brush it on an ultra-white blank brick and put it into an oven for drying.

[0088] Step 7: The dried ultra-white green bricks are kept at 950° C. in an electric furnace at a heating rate of 13° C. / min for 20 min to obtain ceramic bricks covered with a functional coating.

[0089] The performance parameter test results of the aluminum phosphate materials with high radiation performance in the atmospheric window prepared in Examples 1-6 are shown in Table 1 below.

[0090]

[0091] From the test results of the above embodiments, it can be seen that the present invention provides a method for preparing an aluminum phosphate material with high radiation performance in the atmospheric window. After preparing a MOF precursor by a hydrothermal method, a monoclinic aluminum phosphate material is synthesized at a certain temperature, and its morphology and structure are controllable. The process flow of the preparation of the present invention is simple, the raw materials are common, the controllability is strong, and the output is large, and it is easy to realize industrial production. The synthesized monoclinic aluminum phosphate powder has both high solar reflectivity and high and medium infrared emissivity; it can not only reflect the strong heat from the sun, but also radiate its own heat to outer space in the form of infrared rays. The application of the powder obtained by the present invention in ceramic glaze has shown excellent cooling effect through actual temperature measurement tests.

[0092] The present invention provides a method for preparing an aluminum phosphate material with high radiation performance at an atmospheric window, and also provides one of the methods for using the aluminum phosphate material with high radiation performance at an atmospheric window, optimizes the composition ratio of the functional layer glaze, and can effectively exert the excellent performance of the aluminum phosphate material with high radiation performance at an atmospheric window; it also optimizes the preparation method of ceramic tiles with functional coatings, further improves the various properties of the prepared ceramic tiles covered with functional coatings, and especially improves their cooling performance, which can increase the cooling effect from about 4°C to about 6°C.

[0093] Although the present invention has been described in detail above using general descriptions and specific embodiments, it will be apparent to those skilled in the art that modifications and improvements may be made based on the present invention. Therefore, such modifications and improvements, which do not depart from the spirit of the present invention, are intended to be within the scope of protection claimed herein.

Claims

1. A method for preparing an aluminum phosphate material having high radiation performance in an atmospheric window, characterized in that: The following steps are involved: (1) Prepare a solution A with an AlCl3·6H2O content of 0.1 to 1 mol / L; add terephthalic acid and 2-aminophthalic acid to N,N-dimethylacetamide, respectively, and stir evenly to obtain a solution B with a terephthalic acid and 2-aminophthalic acid content of 0.1 to 1 mol / L; The solution A is fully stirred with the solution B to obtain solution C, wherein Al 3+ : The molar ratio of phthalic acid: 2-aminophthalic acid is (1~3): (1~3): (1~3); (2) Prepare solution D with the contents of sodium dihydrogen phosphate and ammonium phosphate ranging from 0.1 to 1 mol / L; Add the D solution to the C solution, and stir the mixture at 50-90°C for 2-6 hours to obtain the F solution, wherein the sodium dihydrogen phosphate: ammonium phosphate: Al 3+ The molar ratio is (1~3):(1~3):(1~3); (3) placing the F solution in a microwave ultrasonic ultraviolet reactor and irradiating it with ultraviolet light of 365 nm at a power of 300-600 W for 2-5 h, then transferring the reaction solution to a hydrothermal reactor, placing the hydrothermal reactor containing the reaction solution in an oven, reacting at 100-180° C. for 8-12 h, and cooling to room temperature to obtain a G solution; (4) The G solution is evaporated by a rotary evaporator to collect the product to obtain product H; the product H is placed in a vacuum drying oven at 70-200°C for 2-5 hours to obtain product I; (5) The product I is placed in a muffle furnace, heated to 280-320°C at a rate of 7-9°C / min, and kept warm for 28-32 minutes; then heated to 700-1000°C at a rate of 9-11°C / min, and kept warm for 1-3 hours to obtain product J; the product J is an aluminum phosphate material with high radiation performance in the atmospheric window.

2. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 1, characterized in that: In the step (1), the solution A is fully stirred with the solution B to obtain a solution C, wherein Al 3+ : The molar ratio of phthalic acid: 2-aminophthalic acid is (2~3): (2~3): (2~3).

3. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 1, characterized in that: In the step (2), the D solution is added to the C solution, and the mixture is stirred at a temperature of 70-90°C for 4-6 hours to obtain the F solution, wherein the mixture is sodium dihydrogen phosphate: ammonium phosphate: Al 3+ The molar ratio is (2~3):(2~3):(2~3).

4. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 1, characterized in that: In the step (3), the F solution is placed in a microwave ultrasonic ultraviolet reactor and irradiated with ultraviolet light of a wavelength of 365 nm at a power of 300-600 W for 3-5 hours. The reaction liquid is then transferred to a hydrothermal reactor, and the hydrothermal reactor containing the reaction liquid is placed in an oven, reacted at 130-180° C. for 10-12 hours, and cooled to room temperature to obtain a G solution.

5. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 1, characterized in that: In the step (4), the G solution is evaporated by a rotary evaporator to collect the product to obtain product H; the product H is placed in a vacuum drying oven and dried at 120-200° C. for 3-5 hours to obtain product I.

6. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 1, characterized in that: In the step (5), the product I is placed in a muffle furnace, heated to 300-320°C at a rate of 8-9°C / min, and kept warm for 30-32 min; then heated to 900-1000°C at a rate of 10-11°C / min, and kept warm for 2-3 h to obtain product J; the product J is an aluminum phosphate material with high radiation performance in the atmospheric window.

7. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 1, characterized in that: The method for using the prepared aluminum phosphate material with high radiation performance at the atmospheric window is as follows: 1) weighing 2-5 parts by weight of washed kaolin, 30-40 parts by weight of frit, 1-4 parts by weight of sodium tripolyphosphate, 3-5 parts by weight of feldspar, and 1-4 parts by weight of the product J; putting them together in a ball mill and ball milling them; passing the ball-milled slurry through a 200-mesh sieve to obtain a functional layer glaze; 2) applying the functional layer glaze to ultra-white green bricks, drying, and firing to obtain ceramic tiles covered with a functional coating.

8. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 7, characterized in that: The method for using the prepared aluminum phosphate material with high radiation performance at the atmospheric window is as follows: 1) weighing 3-5 parts by weight of washed kaolin, 35-40 parts by weight of frit, 3-4 parts by weight of sodium tripolyphosphate, 4-5 parts by weight of feldspar, and 3-4 parts by weight of the product J; putting them together in a ball mill and ball milling them; passing the ball-milled slurry through a 200-mesh sieve to obtain a functional layer glaze; 2) applying the functional layer glaze to ultra-white green bricks, drying, and firing to obtain ceramic tiles covered with a functional coating.

9. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 7, characterized in that: In the step 2), the functional layer glaze is applied to the ultra-white blank brick, and the brick is placed in an oven for drying to obtain a dried ultra-white blank brick; the dried ultra-white blank brick is placed in an electric furnace, heated to 800-1000°C at a heating rate of 7-10°C / min, and kept warm for 18-22 minutes to obtain a ceramic brick covered with a functional coating.

10. The method for preparing an aluminum phosphate material having high radiation performance at an atmospheric window according to claim 9, characterized in that: In the step 2), the functional layer glaze is applied to the ultra-white blank brick, and the brick is placed in an oven for drying to obtain a dried ultra-white blank brick; the dried ultra-white blank brick is placed in an electric furnace, heated to 950-1000°C at a heating rate of 8-10°C / min, and kept warm for 20-22 minutes to obtain a ceramic brick covered with a functional coating.

Images