CN110746882B - Preparation method of high-spectrum selective absorption solar photo-thermal conversion coating - Google Patents
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/20—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption
- F24S70/225—Details of absorbing elements characterised by absorbing coatings; characterised by surface treatment for increasing absorption for spectrally selective absorption
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- F24S70/00—Details of absorbing elements
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Abstract
A preparation method of a high-spectrum selective absorption solar photo-thermal conversion coating belongs to the technical field of new energy materials. The invention utilizes one or two of copper acetate or copper nitrate, one or two of manganese acetate or manganese chloride and CoCl2·3H2One or two of O, hydroxymethyl cellulose or hydroxypropyl cellulose are taken as raw materials to synthesize CoCuMnOxThe functional filler is prepared by preparing polystyrene microspheres with hydroxyl on the surface as a pore-forming agent, mixing the filler, the pore-forming agent and matrix resin (water-based heat-resistant organic silicon resin), and coating a carrier, wherein the obtained coating has good solar energy absorption selectivity. The solar energy absorbing coating prepared by the invention achieves the same high absorption and low emission effects as the Cr series solar energy coating on the market, and can replace the Cr series solar energy absorbing coating on the market.
Description
Technical Field
The invention relates to a preparation method of a high-spectrum selective absorption solar photo-thermal conversion coating, and belongs to the technical field of new energy materials.
Background
The solar energy absorbing paint has visible light band emissivity near zero and infrared light band emissivity near 1, can selectively absorb solar energy, and is suitable for coating solar heat collector with low temperature. The solar energy absorption coating is used as a new energy material and has good market prospect.
Solar energy absorption coating has a great influence on the technical and economic performance of solar energy utilization, and in order to improve the utilization rate of solar energy devices and reduce the cost, solar energy science and technology workers in various countries pay attention to research and development of solar energy absorption coatings, develop various coatings, and some of the coatings are already used for production, so that a good effect is achieved. The electroplating coating is a mature technology of solar energy absorbing materials and is divided into a black chromium coating or a black nickel coating, the absorption ratio alpha and the emission ratio epsilon of the black chromium coating are respectively 0.93-0.97 and 0.07-0.15, the alpha/epsilon is 6-13, and the electroplating coating has excellent spectral selectivity. The black chromium coating has good thermal stability and high temperature resistance, is suitable for high temperature conditions, and can stably work for a long time at 300 ℃. In addition, the black chromium coating also has better weather resistance and corrosion resistance. However, the current density of the current black chromium electroplating process is high (15-200A/dm)2) The solution has poor conductivity, generates a large amount of joule heat during electroplating, and needs cooling and ventilation and exhaust to maintain normal production. In addition, the black chromium is plated on the non-copper part, and the production cost is high because copper is pre-plated, bright nickel is plated, and black chromium is plated at last.
The black nickel coating is mostly a nickel alloy coating, the composition of which varies with the plating bath composition and deposition conditions. The black nickel plating solutions are classified into zinc sulfate plating solutions and molybdate-containing plating solutions. The black nickel coating obtained from the first plating solution contains 40-60% of nickel and about 20-30% of zinc. The absorption ratio alpha of the black nickel coating can reach 0.93-0.96, the thermal emission ratio epsilon is 0.08-0.15, alpha/epsilon is close to 6-12, and the absorption performance is good. The black nickel coating is very thin, and in order to improve the binding force and corrosion resistance of the coating and a substrate, an intermediate coating (such as Ni, Cu and Cd) or a double-layer nickel coating is often adopted. The black nickel coating is poor in thermal stability and corrosion resistance, so that the black nickel coating is only suitable for low-temperature solar heat utilization. With the development of science and technology, there are also technologies such as electrochemical surface conversion coating, vacuum coating and coating type coating, and the coating type solar absorption coating is a diffuse optical surface and consists of two parts of pigment and binder.
The traditional solar heat-absorbing coating mainly takes chromium fillers as main materials, and the chromium fillers mainly take chromium nitrides or chromium oxides as main materials in the existing form, so that the traditional solar heat-absorbing coating has ideal forbidden bandwidth, can highly absorb light in visible-near infrared region wave bands in sunlight, realizes low emission in middle and far infrared wave bands, and is a good solar energy absorbing material. With the increasing environmental protection requirement in recent years, Cr is produced in the process of producing coating3+The requirement for discharging waste water is getting more and more strict, so the demand for researching the solar energy absorption filler for replacing chromium series is urgent.
Disclosure of Invention
The invention aims to provide a preparation method of a high-spectrum selective absorption solar photo-thermal conversion coating, which selects proper transition metal element synthetic composite oxide powder to replace chromium solar absorption coating filler, and increases the surface roughness of the coating through a pore-making agent, thereby increasing diffuse reflection to improve the effective absorption of light.
The technical scheme of the invention is that one or two of copper acetate or copper nitrate, one or two of manganese acetate or manganese chloride and CoCl are utilized2·3H2One or two of O, hydroxymethyl cellulose or hydroxypropyl cellulose are taken as raw materials to synthesize CoCuMnOxThe functional filler is used for preparing polystyrene microspheres with hydroxyl on the surface as a pore-forming agent, and the filler, the pore-forming agent and matrix resin (water-based heat-resistant organic silicon resin) are mixed to prepare the solar selective absorption coating.
A preparation method of a high-spectrum selective absorption solar photo-thermal conversion coating comprises the following steps:
（1）CoCuMnOxpreparing functional filler: taking one or two of copper acetate or copper nitrate, one or two of manganese acetate or manganese chloride and CoCl2·3H2One or two of O, hydroxymethyl cellulose or hydroxypropyl cellulose and water are prepared into a mixed solution;
(2) hole making reaction: dropwise adding polystyrene microspheres into the mixed solution obtained in the step (1), and reacting at a certain temperature;
(3) sol preparation: adding water-based organic silicon resin after the reaction in the step (2), uniformly stirring, and standing to form sol;
(4) coating of a coating: placing the cleaned carrier in the sol prepared in the step (3), and slowly lifting to leave a uniform coating on the carrier;
(5) and (3) post-treatment: and (4) drying the coating carrier obtained in the step (4), then placing the dried coating carrier in a tubular furnace for curing, and taking out the cured coating carrier after annealing to obtain the black solar energy absorption coating on the carrier.
The method comprises the following specific steps in parts by weight:
（1）CoCuMnOxpreparing functional filler: taking 5-10 parts of one or two of copper acetate or copper nitrate, 6-10 parts of one or two of manganese acetate or manganese chloride and CoCl2·3H2CoCuMnO is prepared by 6-12 parts of O7-15 parts, one or two of hydroxymethyl cellulose and hydroxypropyl cellulose and 100 parts of waterxFunctional filler;
(2) hole making reaction: for the CoCuMnO obtained in the step (1)xDripping 3-8 parts of polystyrene microspheres into the functional filler, and reacting at 75-85 ℃ for 1-2 h;
(3) sol preparation: adding 28-35 parts of water-based organic silicon resin after the reaction in the step (2), uniformly stirring, and standing to form sol;
(4) coating of a coating: placing the cleaned carrier in the sol prepared in the step (3), and slowly pulling at the speed of 1mm/s to leave a uniform coating on the carrier;
(5) and (3) post-treatment: and (4) drying the coating carrier obtained in the step (4) at 100 ℃, then placing the dried coating carrier in a tubular furnace to be cured for 4 hours at 300-400 ℃, and taking out the coating carrier after annealing for 12 hours to obtain the high-spectrum selective absorption solar photo-thermal conversion coating on the carrier.
The carrier is a tin plate.
The preparation method of the polystyrene microsphere comprises the following steps:
(1) mixing: uniformly stirring and mixing polyvinylpyrrolidone, absolute ethyl alcohol and deionized water, introducing nitrogen, blowing bubbles, emptying, and heating for reaction;
(2) reaction: after the temperature of the system is stable, adding a certain amount of a mixture of styrene and azobisisobutyronitrile into the reaction system in the step (1); after reacting for a certain time, adding hydroxyethyl methacrylate, continuing to react, and cooling to obtain a white emulsion product;
(3) and (3) post-treatment: centrifuging and settling the white emulsion obtained by the reaction in the step (2), pouring out supernatant, adding absolute ethyl alcohol, performing ultrasonic dispersion, and centrifuging again; repeating the steps for a plurality of times, and taking a sedimentation product;
(4) and (3) drying: and (4) drying the settled product obtained in the step (3) in vacuum at normal temperature to obtain a white solid, namely the polystyrene microsphere.
The preparation of the polystyrene microsphere comprises the following specific steps in parts by weight:
(1) mixing: taking 1-3 parts of polyvinylpyrrolidone, 60-75 parts of absolute ethyl alcohol and 3-5 parts of deionized water as raw materials, stirring at the speed of 130r/min to form a homogeneous system, introducing nitrogen, blowing bubbles, evacuating for 20min, and then starting a temperature control system to rapidly heat the system to 70 ℃;
(2) reaction: when the temperature of the system is stable, adding 10-20 parts of styrene and 0.1-0.2 part of azobisisobutyronitrile into the reaction system in the step (1), and keeping the stirring speed and the nitrogen atmosphere; after reacting for 14h, adding 3-5 parts of hydroxyethyl methacrylate, continuing to react for 10h, and cooling to obtain a white emulsion product;
(3) and (3) post-treatment: centrifuging and settling the white emulsion obtained by the reaction in the step (2) at the rotating speed of 5000r/min, pouring out supernatant, adding 50mL of absolute ethyl alcohol, ultrasonically dispersing for 15min at 40k-42kHz, centrifuging again, and repeating the step for 4-6 times;
(4) and (3) drying: and (4) drying the product obtained in the step (3) in vacuum at the normal temperature of 0.04-0.06MPa to obtain a white solid, namely the polystyrene microsphere.
The solar energy absorptivity of the coating prepared by the invention is 92-95%, and the emissivity is 19-24%.
The invention has the beneficial effects that: the solar energy absorbing coating prepared by the invention has good solar energy absorbing selectivity, achieves the same high-absorption and low-emission effects as the Cr series solar energy coating on the market, and can replace the Cr series solar energy absorbing coating on the market.
Drawings
FIG. 1 is a graph of the spectral reflectance of the coating obtained in example 1.
Detailed Description
Example 1
Preparing a pore-forming agent polystyrene microsphere:
(1) mixing: mixing 1.81g of polyvinylpyrrolidone, 75g of anhydrous ethanol and 5g of deionized water, adding the mixture into a 500mL three-port reaction kettle, stirring at the speed of 130r/min to form a homogeneous system, introducing nitrogen, blowing bubbles, emptying for 20min, and then starting a temperature control system to rapidly heat the system to 70 ℃;
(2) reaction: when the temperature of the system is stable, adding a mixture of 18.1g of styrene and 0.18g of azobisisobutyronitrile, keeping the stirring speed and the nitrogen atmosphere, when the reaction is carried out for 14 hours, adding 4.3g of hydroxyethyl methacrylate once, continuing the reaction for 10 hours, stopping the reaction, and naturally cooling to obtain a white emulsion product;
(3) and (3) post-treatment: carrying out centrifugal sedimentation on the white emulsion obtained by the reaction at the rotating speed of 5000r/min, pouring out supernatant, adding 50mL of absolute ethyl alcohol, carrying out ultrasonic dispersion for 15min, and then centrifuging; and repeating the operation for 5 times to remove unreacted monomers, the dispersion stabilizer and the functional monomers, and finally, drying the obtained product in vacuum for 24 hours at normal temperature to obtain a white solid, namely the polystyrene microsphere with hydroxyl on the surface.
Preparing a high-spectrum selective solar energy absorption photo-thermal conversion coating:
（1）CoCuMnOxpreparing functional filler: taking 8g of copper acetate, 6.92g of manganese acetate and 14.72g of CoCl2·3H2O, 8.72g of hydroxymethyl cellulose and 100g of deionized water are prepared into a mixed solution in a 500mL three-neck flask, and the mixed solution is prepared into CoCuMnOxFunctional filler;
(2) hole making reaction: adding 3-8g of prepared polystyrene microspheres into a flask, and reacting for 1h at 80 ℃;
(3) sol preparation: after the reaction is finished, 35g of water-based organic silicon resin is added, the solution is poured into a beaker to stand for 3 days after being stirred for 30min, and sol is formed;
(4) coating of a coating: placing the cleaned tin plate into the sol, and slowly lifting the tin plate at the speed of 1mm/s by using a lifting machine to ensure that an even coating is left on the iron plate;
(5) and (3) post-treatment: and (3) baking the sample in a baking oven at 100 ℃ for 1h, taking out the sample, putting the sample in a tube furnace, curing the sample for 4h at 400 ℃, and taking out the sample after annealing for 12h to obtain the black solar energy absorbing coating on the tin plate.
The spectral reflectance of the resulting coating is shown in detail in FIG. 1. The prepared solar energy absorbing coating has high-efficiency selectivity, namely the reflectivity of 200-25000 nm is lower than 10%, the reflectivity of 4000-25000nm is higher than 80%, the absorptivity is 93%, the emissivity is 23% according to the formula of absorptivity and emissivity, and the high-absorption and low-emission effects which are the same as those of the Cr series solar coating on the market are achieved.
Claims (4)
1. A preparation method of a high-spectrum selective absorption solar photo-thermal conversion coating is characterized by comprising the following steps: the solar absorptivity of the coating is 92% -95%, and the emissivity is 19% -24%; the method comprises the following steps:
（1）CoCuMnOxpreparing functional filler: taking 5-10 parts of one or two of copper acetate or copper nitrate, 6-10 parts of one or two of manganese acetate or manganese chloride and CoCl2·3H2CoCuMnO is prepared by 6-12 parts of O7-15 parts, one or two of hydroxymethyl cellulose and hydroxypropyl cellulose and 100 parts of waterxFunctional filler;
(2) hole making reaction: for the CoCuMnO obtained in the step (1)xDripping 3-8 parts of polystyrene microspheres into the functional filler, and reacting at 75-85 ℃ for 1-2 h;
(3) sol preparation: adding 28-35 parts of water-based organic silicon resin after the reaction in the step (2), uniformly stirring, and standing to form sol;
(4) coating of a coating: placing the cleaned carrier in the sol prepared in the step (3), and slowly pulling at the speed of 1mm/s to leave a uniform coating on the carrier;
(5) and (3) post-treatment: and (4) drying the coating carrier obtained in the step (4) at 100 ℃, then placing the dried coating carrier in a tubular furnace to be cured for 4 hours at 300-400 ℃, and taking out the coating carrier after annealing for 12 hours to obtain the high-spectrum selective absorption solar photo-thermal conversion coating on the carrier.
2. The preparation method of the high-spectral selective absorption solar photo-thermal conversion coating according to claim 1, which is characterized by comprising the following steps: the carrier is a tin plate.
3. The preparation method of the solar energy photo-thermal conversion coating with high spectral selectivity absorption according to claim 1, wherein the preparation method of the polystyrene microsphere is as follows:
(1) mixing: uniformly stirring and mixing polyvinylpyrrolidone, absolute ethyl alcohol and deionized water, introducing nitrogen, blowing bubbles, emptying, and heating for reaction;
(2) reaction: after the temperature of the system is stable, adding a certain amount of a mixture of styrene and azobisisobutyronitrile into the reaction system in the step (1); after reacting for a certain time, adding hydroxyethyl methacrylate, continuing to react, and cooling to obtain a white emulsion product;
(3) and (3) post-treatment: centrifuging and settling the white emulsion obtained by the reaction in the step (2), pouring out supernatant, adding absolute ethyl alcohol, performing ultrasonic dispersion, and centrifuging again; repeating the steps for a plurality of times, and taking a sedimentation product;
(4) and (3) drying: and (4) drying the settled product obtained in the step (3) in vacuum at normal temperature to obtain a white solid, namely the polystyrene microsphere.
4. The preparation method of the solar energy photo-thermal conversion coating with high spectral selectivity absorption according to claim 3, which is characterized in that the preparation method of the polystyrene microsphere comprises the following specific steps in parts by weight:
(1) mixing: taking 1-3 parts of polyvinylpyrrolidone, 60-75 parts of absolute ethyl alcohol and 3-5 parts of deionized water as raw materials, stirring at the speed of 130r/min to form a homogeneous system, introducing nitrogen, blowing bubbles, evacuating for 20min, and then starting a temperature control system to rapidly heat the system to 70 ℃;
(2) reaction: when the temperature of the system is stable, adding 10-20 parts of styrene and 0.1-0.2 part of azobisisobutyronitrile into the reaction system in the step (1), and keeping the stirring speed and the nitrogen atmosphere; after reacting for 14h, adding 3-5 parts of hydroxyethyl methacrylate, continuing to react for 10h, and cooling to obtain a white emulsion product;
(3) and (3) post-treatment: centrifuging and settling the white emulsion obtained by the reaction in the step (2) at the rotating speed of 5000r/min, pouring out supernatant, adding 50mL of absolute ethyl alcohol, ultrasonically dispersing for 15min at 40k-42kHz, centrifuging again, and repeating the step for 4-6 times;
(4) and (3) drying: and (4) drying the product obtained in the step (3) in vacuum at the normal temperature of 0.04-0.06MPa to obtain a white solid, namely the polystyrene microsphere.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103046048A (en) * | 2012-12-28 | 2013-04-17 | 郝勇 | Method for preparing medium and high temperature solar selective absorbing coating by using sol-gel method |
| CN106298246A (en) * | 2016-08-05 | 2017-01-04 | 宁波高智科技咨询服务有限公司 | A kind of preparation method of solar cell surface influx and translocation layer |
| CN108359375A (en) * | 2018-01-31 | 2018-08-03 | 武汉理工大学 | A kind of high temperature solar selectively absorbing coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103046048A (en) * | 2012-12-28 | 2013-04-17 | 郝勇 | Method for preparing medium and high temperature solar selective absorbing coating by using sol-gel method |
| CN106298246A (en) * | 2016-08-05 | 2017-01-04 | 宁波高智科技咨询服务有限公司 | A kind of preparation method of solar cell surface influx and translocation layer |
| CN108359375A (en) * | 2018-01-31 | 2018-08-03 | 武汉理工大学 | A kind of high temperature solar selectively absorbing coating and preparation method thereof |
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| Title |
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| 多孔结构高吸收涂层的制备与性能研究;王泽江;《中国优秀硕士学位论文全文数据库工程科技Ⅱ辑》;20180215(第02期);第46页第5.2节第1段-第2段、第59页第3段-60页最后一段 * |
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