CN115260821A - Transparent heat-insulating coating with microstructure and preparation method and application thereof - Google Patents

Transparent heat-insulating coating with microstructure and preparation method and application thereof Download PDF

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CN115260821A
CN115260821A CN202210852048.XA CN202210852048A CN115260821A CN 115260821 A CN115260821 A CN 115260821A CN 202210852048 A CN202210852048 A CN 202210852048A CN 115260821 A CN115260821 A CN 115260821A
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microstructure
coating
preparation
ball milling
transparent heat
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李萍
程锹轩
王锦新
向建化
陈华金
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Guangzhou University
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Guangzhou University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/004Reflecting paints; Signal paints
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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Abstract

The invention provides a transparent heat insulation coating with a microstructure and a preparation method and application thereof. The preparation method of the transparent heat insulation coating with the microstructure comprises the following steps: s1: mixing deionized water, a dispersing agent and nano powder, and then carrying out ball milling to prepare slurry; s2: mixing the slurry with a UV curing agent, and then carrying out ball milling to prepare a coating; s3: and coating the coating on the substrate by using a wire rod with a microstructure, and curing and forming to obtain the transparent heat-insulating coating with the microstructure. The transparent heat-insulating coating disclosed by the invention is simple in preparation method and low in manufacturing cost, can be produced in large scale in batch, and is high in visible light transmittance and excellent in cooling and heat-insulating effects.

Description

Transparent heat-insulating coating with microstructure and preparation method and application thereof
Technical Field
The invention relates to the technical field of heat insulation coatings, in particular to a transparent heat insulation coating with a microstructure and a preparation method and application thereof.
Background
Sustainable development and green development are mainstream of future development, and reducing energy consumption and saving energy are main measures of sustainable development and green development in China. The energy consumption of China in the building industry accounts for about 35 percent of the total consumption of China. In summer and winter, the use of air conditioners and heating accounts for 40% of the energy consumption of a building. In order to reduce energy consumption, a layer of transparent heat insulation coating can be coated on the building glass and the outer wall, the transparent heat insulation coating effectively reduces the temperature and reduces the thermal sensation brought by infrared light, and therefore the use of an air conditioner is reduced.
The heat insulation principle of the existing transparent heat insulation coating is to reflect near infrared light and reduce the heat effect of the infrared light, but the visible light transmittance of the existing transparent heat insulation coating is still low. Meanwhile, the thickness of the transparent heat insulation coating is too thin, so that the near-infrared reflection effect is reduced, and the heat insulation effect is influenced; the thickness of the transparent heat insulation coating is too thick, and the visible light transmittance is reduced. However, glass is adopted in many buildings in China, the low visible light transmittance can affect the appearance and reduce the utilization of solar energy, and particularly when the glass is applied to photovoltaic power generation, the low visible light transmittance can affect the photoelectric conversion efficiency.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a transparent heat insulation coating with a microstructure, and a preparation method and application thereof.
The invention provides a preparation method of a transparent heat insulation coating with a microstructure, which comprises the following steps:
s1: mixing deionized water, a dispersing agent and nano powder, and then carrying out ball milling to prepare slurry;
s2: mixing the slurry with a UV curing agent, and then carrying out ball milling to prepare a coating;
s3: and coating the coating on the substrate by adopting a wire rod with a microstructure, and curing and forming to obtain the transparent heat-insulating coating with the microstructure.
In the invention, the nano powder can be prepared into a coating by uniformly dispersing the nano powder which is low in price, can transmit visible light and can shield near infrared light, and the visible light can be effectively transmitted and the near infrared light can be effectively reflected. Specifically, the materials for shielding the visible light high-transmittance near-infrared light can be cesium tungsten bronze, indium tin oxide, nano ATO and the like, and the materials have the characteristics of high visible light transmittance and near-infrared light reflection; the nano ATO is relatively low in price, good in visible light transmission performance and not easy to generate heat accumulation, so that the nano ATO is preferably used as the nano powder. The particle size of the nanopowder is not particularly limited, and may be, for example, 40 to 60nm.
The uniform dispersion of the nano powder is an important index for preparing the slurry, and if the nano powder is not uniformly dispersed, the slurry is agglomerated, and the transmittance of visible light is affected. The preparation method adopts a mode of combining physical dispersion with chemical dispersion to prepare the slurry with uniform distribution, wherein the physical dispersion is dispersed by a ball mill, the chemical dispersion is dispersed by a dispersing agent, and the dispersing agent can adopt a silane coupling agent, such as a silane coupling agent KH560 and the like. Adding the nano ATO powder, deionized water and a silane coupling agent KH560 into a ball milling tank, starting a ball mill for ball milling, and preparing the slurry with uniformly dispersed nano ATO powder.
During ball milling, the dosage proportion of deionized water, a dispersing agent and nano powder can be controlled to be (140-160) mL: (5-10) g: (1-3) g. In addition, ball milling can be carried out by adopting ball milling beads with the diameter of 0.1-0.3mm, and the ball-to-material ratio can be controlled to be (6-8): (2-4), the rotating speed is 400-500r/min, the ball milling time is 4-6h, and the material of ball milling beads can be zirconium dioxide and the like; wherein, the ball material ratio refers to the volume ratio of the ball milling beads to the mixed material of the deionized water, the dispersant and the nano powder.
In the present invention, a UV curing agent having transparency and high visible light transmittance, for example, a UV curing agent K2018 or the like, may be selected. The curing agent has excellent wear resistance and acid and alkali resistance, and the prepared coating is tough, firm in bonding and high in visible light transmittance; meanwhile, the UV curing agent K2018 can be used for glass, and the UV curing agent K2018 and the slurry are placed into a ball milling tank for ball milling to obtain the coating. During ball milling, the volume ratio of the slurry to the UV curing agent can be 1: (1.5-2.5), in addition, ball milling beads with the diameter of 0.1-0.3mm can be adopted for ball milling, and the ball-to-material ratio can be controlled to be (6-8): (2-4), the rotating speed is 400-500r/min, the ball milling time is 4-6h, and the material of the ball milling beads can be zirconium dioxide and the like.
In the present invention, an optical glass which is inexpensive and has high transmittance in visible light can be selected as the substrate. In order to make full use of sunlight and have a better visible light transmittance, optical glass having a high visible light transmittance may be selected as the substrate. Since the high and low transmittance of visible light directly affects the utilization efficiency of sunlight, in order to fully utilize sunlight, the substrate may be optical glass K9 or optical glass BK7, which has high hardness, good scratch resistance and high transmittance of visible light, and preferably optical glass BK7.
In the present invention, the microstructure may be a V-groove microstructure; preferably, the vertex angle of the V-shaped groove microstructure can be 60-80 degrees, and the structure period is 25-35 μm. Specifically, a CNC (computerized numerical control) precision grinder can be used for processing an array V-shaped groove microstructure on a bar, and the processed microstructure bar is polished and cleaned for later use.
The invention also provides a transparent heat insulation coating with a microstructure, which is prepared according to the preparation method.
The invention also provides application of the transparent heat insulation coating with the microstructure in building glass or an outer wall.
The transparent heat insulation coating has a microstructure, the microstructure has a good antireflection effect, and the transmittance of visible light can be effectively increased; the existing microstructure coating preparation process usually adopts a nanoimprint method to carry out repeated etching, and transfers the microstructure on a template to a material to be processed by the assistance of photoresist, and the processing method has extremely high requirements on processing equipment and relatively expensive processing cost; the microstructure is processed on the wire rod, the special coating is coated on the substrate by the wire rod with the microstructure for film coating processing, the transparent heat insulation coating with the microstructure can be obtained, and the microstructure coating is irradiated by the UV curing lamp for curing, so that the transparent heat insulation coating with the microstructure can be prepared.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of a bar having a V-groove microstructure according to one embodiment;
FIG. 2 is a schematic diagram of a bar coater having a V-groove microstructure according to an embodiment;
FIG. 3 is a process diagram of one embodiment of a transparent thermal barrier coating having microstructures;
FIG. 4 is a graph of the transmittance of a transparent thermal barrier coating prepared in example 1; wherein: a is a V-shaped groove microstructure transparent heat insulation coating; and B is a transparent heat-insulating coating without a microstructure.
Description of reference numerals:
1: a V-shaped groove microstructure wire rod; 2: a V-shaped groove microstructure wire rod film coating device; 3: a BK7 optical glass substrate; 4: transparent heat insulation coating; 5: a V-shaped groove microstructure transparent heat insulation coating; 6: a UV curing lamp.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms also include the plural forms unless the context clearly dictates otherwise, and further, it is understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, devices, components, and/or combinations thereof.
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1 to 3, the method for preparing the transparent thermal barrier coating with the microstructure according to the embodiment includes the following steps:
1. preparation of V-groove microstructure wire rod 1
Firstly, trimming a grinding wheel, trimming the vertex angle of the grinding wheel into a V shape of 70 degrees, fixing a 20cm wire rod on a processing table, setting the rough grinding depth to be 0.08 mm, setting the rotation speed of the rough grinding wheel to be 2500 rpm, setting the rough grinding feed speed to be 600 mm/min and setting the rough grinding feed depth to be 0.002 mm; the finish grinding depth is 0.002 mm, the rotation speed of the finish grinding wheel is 4000 rpm, the finish grinding feed speed is 100 mm/min, the finish grinding feed depth is 0.001 mm, the rough grinding V-shaped tip grinding wheel is a #600 metal-based diamond grinding wheel, and the finish grinding V-shaped tip grinding wheel is a #3000 resin-based diamond grinding wheel. Through the processing, the V-shaped groove microstructure bar 1 with the apex angle of 70 degrees and the structure period of 30 mu m is obtained.
2. Preparation of nano ATO slurry
Taking 150mL of deionized water, 8g of 50nm ATO nano powder and 2g of silane coupling agent KH560, putting the mixed material and 0.2mm zirconium dioxide ball-milling beads into a ball-milling tank, stirring and mixing, wherein the volume ratio of the mixed material to the ball-milling beads is 3:7. and starting the ball mill, setting the rotating speed to be 500r/min, and carrying out ball milling for 4 hours to obtain the slurry with uniformly dispersed nano ATO powder.
3. Preparation of the coating
Mixing the UV curing agent K2018 with the slurry according to the weight ratio of 2: adding the mixture into a ball milling tank according to the volume ratio of 1, and continuing ball milling for 4 hours to obtain a transparent heat insulation coating 4.
4. Preparation of transparent thermal barrier coating
The BK7 optical glass substrate 3 is cleaned to remove oil stains on the surface of the glass substrate, so that the BK7 optical glass substrate 3 is in a pollution-free, dust-free and ion-free state.
The clean BK7 optical glass substrate 3 is placed in a plane workbench to be fixed, a processed V-shaped groove microstructure wire rod 1 is installed, the prepared transparent heat insulation coating 4 is sampled and placed on the BK7 optical glass substrate 3, a film is coated on the BK7 optical glass substrate 3 by using a V-shaped groove microstructure wire rod coating device 2, after the film coating is finished, the film is immediately irradiated by a UV curing lamp 6 to be cured and formed, and the V-shaped groove microstructure transparent heat insulation coating 5 is prepared, wherein the transmissivity curve of the V-shaped groove microstructure transparent heat insulation coating is shown in figure 1.
Example 2
The preparation method of the transparent thermal insulation coating with the microstructure of the embodiment comprises the following steps:
1. micro-structure wire rod for preparing V-shaped groove
Firstly, trimming a grinding wheel, trimming the vertex angle of the grinding wheel into a V shape of 60 degrees, fixing a 20cm wire rod on a processing table, setting the rough grinding depth to be 0.08 mm, setting the rotation speed of the rough grinding wheel to be 2500 rpm, setting the rough grinding feed speed to be 600 mm/min and setting the rough grinding feed depth to be 0.002 mm; the finish grinding depth is 0.002 mm, the rotation speed of the finish grinding wheel is 4000 revolutions per minute, the feed speed of the finish grinding is 100 mm per minute, the feed depth of the finish grinding is 0.001 mm, the rough grinding V-shaped tip grinding wheel is a #600 metal-based diamond grinding wheel, and the finish grinding V-shaped tip grinding wheel is a #3000 resin-based diamond grinding wheel. Through the processing, the V-shaped groove microstructure wire rod with the apex angle of 60 degrees and the structure period of 25 mu m is obtained.
2. Preparation of nano ATO slurry
Taking 160mL of deionized water, 40nm of ATO nano powder 10g and 3g of silane coupling agent KH560, putting the mixed material and 0.1mm of zirconium dioxide ball-milling beads into a ball-milling tank, stirring and mixing, wherein the volume ratio of the mixed material to the ball-milling beads is 2:8. and starting the ball mill, setting the rotating speed to be 450r/min, and carrying out ball milling for 5 hours to obtain the slurry with uniformly dispersed nano ATO powder.
3. Preparation of the coating
Mixing the UV curing agent K2018 with the slurry according to the weight ratio of 1.5: adding the mixture into a ball milling tank according to the volume ratio of 1, and continuing ball milling for 5 hours to obtain the transparent heat insulation coating.
4. Preparation of a transparent thermal barrier coating
And cleaning the BK7 optical glass substrate to remove oil stains on the surface of the glass substrate, so that the BK7 optical glass substrate is in a state of no pollution, no dust and no ions.
The clean BK7 optical glass substrate is placed in a plane workbench to be fixed, a processed V-shaped groove microstructure line bar is installed, the prepared transparent heat insulation coating is sampled and placed on the BK7 optical glass substrate, a film is coated on the BK7 optical glass substrate by using a V-shaped groove microstructure line bar film coating device, and after the film coating is finished, the V-shaped groove microstructure line bar film coating device is immediately irradiated by a UV curing lamp to be cured and formed, so that the V-shaped groove microstructure transparent heat insulation coating is prepared.
Example 3
The preparation method of the transparent thermal insulation coating with the microstructure of the embodiment comprises the following steps:
1. micro-structure wire rod for preparing V-shaped groove
Firstly, trimming a grinding wheel, trimming the vertex angle of the grinding wheel into a V shape of 80 degrees, fixing a 20cm wire rod on a processing table, setting the rough grinding depth to be 0.08 mm, setting the rotation speed of the rough grinding wheel to be 2500 rpm, setting the rough grinding feed speed to be 600 mm/min and setting the rough grinding feed depth to be 0.002 mm; the finish grinding depth is 0.002 mm, the rotation speed of the finish grinding wheel is 4000 rpm, the finish grinding feed speed is 100 mm/min, the finish grinding feed depth is 0.001 mm, the rough grinding V-shaped tip grinding wheel is a #600 metal-based diamond grinding wheel, and the finish grinding V-shaped tip grinding wheel is a #3000 resin-based diamond grinding wheel. Through the processing, the V-shaped groove microstructure wire rod with the apex angle of 80 degrees and the structure period of 35 mu m is obtained.
2. Preparation of Nano ATO slurry
Taking 140mL of deionized water, 5g of 60nm ATO nano powder and 1g of silane coupling agent KH560, putting the mixed material and 0.3mm zirconium dioxide ball milling beads into a ball milling tank, stirring and mixing, wherein the volume ratio of the mixed material to the ball milling beads is 4:6. and starting the ball mill, setting the rotating speed to be 400r/min, and performing ball milling for 6 hours to obtain the slurry with uniformly dispersed nano ATO powder.
3. Preparation of the coating
Mixing the UV curing agent K2018 with the slurry according to the proportion of 2.5:1, and continuously ball-milling for 6 hours to obtain the transparent heat-insulating coating.
4. Preparation of transparent thermal barrier coating
The BK7 optical glass substrate is cleaned, and oil stains on the surface of the glass substrate are washed away, so that the BK7 optical glass substrate is free of pollution, dust and ions.
The clean BK7 optical glass substrate is placed in a plane workbench to be fixed, a processed V-shaped groove microstructure line bar is installed, the prepared transparent heat insulation coating is sampled and placed on the BK7 optical glass substrate, a film is coated on the BK7 optical glass substrate by using a V-shaped groove microstructure line bar film coating device, and after the film coating is finished, the V-shaped groove microstructure line bar film coating device is immediately irradiated by a UV curing lamp to be cured and formed, so that the V-shaped groove microstructure transparent heat insulation coating is prepared.
Comparative example 1
The same procedure as in example 1 was repeated except that the coating was carried out using a raw wire bar (i.e., a wire bar having no V-groove microstructure).
Comparative example 2
The bar was substantially the same as example 1 except that the V-groove microstructure bar had a vertex angle of 50 ° and a structure period of 20 μm.
Comparative example 3
The microstructure of the microstructure bar is different, and the other parts are basically the same as the embodiment 1; the microstructure of this comparative example was a U-shaped groove.
Comparative example 4
Except that the dosage of the silane coupling agent KH560 in the step of preparing the nano ATO slurry is 0.5g, and the volume ratio of the UV curing agent K2018 to the slurry in the step of preparing the coating is 3:1, the rest is basically the same as example 1.
Test example 1
The ultraviolet visible near-infrared spectrophotometer is adopted to test the visible light transmittance of each transparent heat insulation coating, and the simulation heat insulation test equipment is adopted to test the cooling and heat insulation effects of each transparent heat insulation coating, and the results are shown in table 1.
TABLE 1 Performance test results of each transparent thermal barrier coating
Transparent thermal barrier coating Transmittance of visible light Near infrared rejection Temperature was measured by irradiating for 10 minutes
Example 1 84.57% 85.32% 49.6°
Example 2 83.78% 84.21% 51.3°
Example 3 83.82% 84.34% 51.2°
Comparative example 1 73.21% 87.86% 49.1°
Comparative example 2 81.32% 83.52% 51.8°
Comparative example 3 79.87% 81.23% 52.4°
Comparative example 4 81.74% 56.92% 57.6°
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A preparation method of a transparent heat insulation coating with a microstructure is characterized by comprising the following steps:
s1: mixing deionized water, a dispersing agent and nano powder, and then carrying out ball milling to prepare slurry;
s2: mixing the slurry with a UV curing agent, and then carrying out ball milling to prepare a coating;
s3: and coating the coating on the substrate by using a wire rod with a microstructure, and curing and forming to obtain the transparent heat-insulating coating with the microstructure.
2. The preparation method according to claim 1, wherein the nanopowder is selected from at least one of cesium tungsten bronze, indium tin oxide and nano ATO, preferably nano ATO.
3. The method according to claim 1, wherein the dispersant is a silane coupling agent, preferably a silane coupling agent KH560.
4. The preparation method of claim 1, wherein the dosage ratio of the deionized water, the nano-powder and the dispersing agent is (140-160) mL: (5-10) g: (1-3) g.
5. The preparation method according to claim 1, characterized in that ball milling is carried out by using ball milling beads with the diameter of 0.1-0.3mm, and the ball milling is carried out by controlling the ball-to-material ratio to be (6-8): (2-4), the rotating speed is 400-500r/min, and the ball milling time is 4-6h.
6. The preparation method according to claim 1, wherein the volume ratio of the slurry to the UV curing agent is 1: (1.5-2.5).
7. The production method according to claim 1, wherein the substrate is an optical glass, preferably an optical glass K9 or an optical glass BK7.
8. The method of claim 1, wherein the microstructure is a V-groove microstructure.
9. A transparent thermal barrier coating having a microstructure, characterized by being produced by the production method according to any one of claims 1 to 8.
10. Use of the transparent thermal barrier coating having a microstructure according to claim 9 in architectural glass or exterior walls.
CN202210852048.XA 2022-07-19 2022-07-19 Transparent heat-insulating coating with microstructure and preparation method and application thereof Pending CN115260821A (en)

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